US2921914A - Preparation of blue colloidal silver dispersions for antihalo layer - Google Patents
Preparation of blue colloidal silver dispersions for antihalo layer Download PDFInfo
- Publication number
- US2921914A US2921914A US639863A US63986357A US2921914A US 2921914 A US2921914 A US 2921914A US 639863 A US639863 A US 639863A US 63986357 A US63986357 A US 63986357A US 2921914 A US2921914 A US 2921914A
- Authority
- US
- United States
- Prior art keywords
- silver
- salt
- gelatin
- blue
- strontium
- 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
- 239000006185 dispersion Substances 0.000 title claims description 18
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title description 13
- 238000002360 preparation method Methods 0.000 title description 4
- 229920000159 gelatin Polymers 0.000 claims description 16
- 239000008273 gelatin Substances 0.000 claims description 16
- 108010010803 Gelatin Proteins 0.000 claims description 15
- 235000019322 gelatine Nutrition 0.000 claims description 15
- 235000011852 gelatine desserts Nutrition 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 15
- 159000000008 strontium salts Chemical class 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- GGCZERPQGJTIQP-UHFFFAOYSA-N sodium;9,10-dioxoanthracene-2-sulfonic acid Chemical compound [Na+].C1=CC=C2C(=O)C3=CC(S(=O)(=O)O)=CC=C3C(=O)C2=C1 GGCZERPQGJTIQP-UHFFFAOYSA-N 0.000 claims description 11
- TUSDEZXZIZRFGC-UHFFFAOYSA-N 1-O-galloyl-3,6-(R)-HHDP-beta-D-glucose Natural products OC1C(O2)COC(=O)C3=CC(O)=C(O)C(O)=C3C3=C(O)C(O)=C(O)C=C3C(=O)OC1C(O)C2OC(=O)C1=CC(O)=C(O)C(O)=C1 TUSDEZXZIZRFGC-UHFFFAOYSA-N 0.000 claims description 10
- 239000001263 FEMA 3042 Substances 0.000 claims description 10
- LRBQNJMCXXYXIU-PPKXGCFTSA-N Penta-digallate-beta-D-glucose Natural products OC1=C(O)C(O)=CC(C(=O)OC=2C(=C(O)C=C(C=2)C(=O)OC[C@@H]2[C@H]([C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)O2)OC(=O)C=2C=C(OC(=O)C=3C=C(O)C(O)=C(O)C=3)C(O)=C(O)C=2)O)=C1 LRBQNJMCXXYXIU-PPKXGCFTSA-N 0.000 claims description 10
- LRBQNJMCXXYXIU-NRMVVENXSA-N tannic acid Chemical compound OC1=C(O)C(O)=CC(C(=O)OC=2C(=C(O)C=C(C=2)C(=O)OC[C@@H]2[C@H]([C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)O2)OC(=O)C=2C=C(OC(=O)C=3C=C(O)C(O)=C(O)C=3)C(O)=C(O)C=2)O)=C1 LRBQNJMCXXYXIU-NRMVVENXSA-N 0.000 claims description 10
- 229940033123 tannic acid Drugs 0.000 claims description 10
- 235000015523 tannic acid Nutrition 0.000 claims description 10
- 229920002258 tannic acid Polymers 0.000 claims description 10
- 230000009467 reduction Effects 0.000 claims description 8
- 229910052709 silver Inorganic materials 0.000 claims description 8
- 239000004332 silver Substances 0.000 claims description 8
- 229910052783 alkali metal Inorganic materials 0.000 claims description 4
- 239000011541 reaction mixture Substances 0.000 claims description 3
- LSNNMFCWUKXFEE-UHFFFAOYSA-N Sulfurous acid Chemical compound OS(O)=O LSNNMFCWUKXFEE-UHFFFAOYSA-N 0.000 claims 1
- 150000001340 alkali metals Chemical class 0.000 claims 1
- DHEQXMRUPNDRPG-UHFFFAOYSA-N strontium nitrate Chemical compound [Sr+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O DHEQXMRUPNDRPG-UHFFFAOYSA-N 0.000 description 12
- QIGBRXMKCJKVMJ-UHFFFAOYSA-N Hydroquinone Chemical compound OC1=CC=C(O)C=C1 QIGBRXMKCJKVMJ-UHFFFAOYSA-N 0.000 description 10
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 10
- 159000000007 calcium salts Chemical class 0.000 description 9
- 229940026236 strontium nitrate Drugs 0.000 description 6
- 239000003638 chemical reducing agent Substances 0.000 description 5
- 238000001246 colloidal dispersion Methods 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- 229960001516 silver nitrate Drugs 0.000 description 5
- 229910001961 silver nitrate Inorganic materials 0.000 description 5
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- -1 alkali metal sulfite Chemical class 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 239000002585 base Substances 0.000 description 2
- 239000000839 emulsion Substances 0.000 description 2
- 239000011640 ferrous citrate Substances 0.000 description 2
- 235000019850 ferrous citrate Nutrition 0.000 description 2
- APVZWAOKZPNDNR-UHFFFAOYSA-L iron(ii) citrate Chemical compound [Fe+2].OC(=O)CC(O)(C([O-])=O)CC([O-])=O APVZWAOKZPNDNR-UHFFFAOYSA-L 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- WYCFMBAHFPUBDS-UHFFFAOYSA-L silver sulfite Chemical compound [Ag+].[Ag+].[O-]S([O-])=O WYCFMBAHFPUBDS-UHFFFAOYSA-L 0.000 description 2
- 235000010265 sodium sulphite Nutrition 0.000 description 2
- 101710134784 Agnoprotein Proteins 0.000 description 1
- 229920001353 Dextrin Polymers 0.000 description 1
- 239000004375 Dextrin Substances 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- VSGNNIFQASZAOI-UHFFFAOYSA-L calcium acetate Chemical compound [Ca+2].CC([O-])=O.CC([O-])=O VSGNNIFQASZAOI-UHFFFAOYSA-L 0.000 description 1
- 239000001639 calcium acetate Substances 0.000 description 1
- 235000011092 calcium acetate Nutrition 0.000 description 1
- 229960005147 calcium acetate Drugs 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 235000019425 dextrin Nutrition 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 150000003378 silver Chemical class 0.000 description 1
- RXSHXLOMRZJCLB-UHFFFAOYSA-L strontium;diacetate Chemical compound [Sr+2].CC([O-])=O.CC([O-])=O RXSHXLOMRZJCLB-UHFFFAOYSA-L 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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
- G03C1/825—Photosensitive materials characterised by the base or auxiliary layers characterised by antireflection means or visible-light filtering means, e.g. antihalation
- G03C1/8255—Silver or silver compounds therefor
Definitions
- the present invention relates to colloidal dispersions of silver which are blue in color, and as such, particularly well adapted for use as antihalation layers for color film.
- colloidal dispersions of silverin aqueous gelatin solutions by reduction of silver salts is a well known process.
- colloidal dispersions have been used in photography as antihalation layers or as filter layers for color film, particularly when located between the upper blue sensitive and the intermediate green sensitive layers of multilayer color film.
- colloidal silver filter layers are recommended for absorbing blue light to prevent exposure thereby of the layers sensitized to the longer wave lengths but which also possess an inherent blue sensitivity.
- the colloidal silver is produced, according to this patent, by the reduction of silver nitrate in an alkaline medium in the presence of a peptizing agent by means of such organic reducing agents as dextrin, ferrous citrate or hydroquinone followedby dispersion in gelatin.
- the quantity of silver used is roughly 30 grams of silver nitrate to 1 kilo of emulsion.
- the blue colored dispersions are particularly desirable for forming antihalation layers on color film for the reason that they are more highly efficient in absorbing the longer wave lengths of light to which the layers adjacent the base are sensitive and by which they would be exposed through light reflected from the surface of the base.
- the critical feature of the patent is the employment, in the reduction, of a calcium salt such as calcium acetate or the like, to which is attributed the ability to obtain large particles without the particles precipitating from the gelatin.
- a calcium salt such as calcium acetate or the like
- the calcium salt must be present in a quantity equal to at least about .0017 mole per liter or reaction mixture.
- Tannic acid operates to much greater advantage than the conventional reducing ag'ents such as dextr in, hydroquinone, ferrous citrate and the like, particularly in the presence of the strontium salt. In fact, my results are directly dependent upon the conjoint-use of tannic acid and strontium salts.
- the procedure contemplated herein involves dissolving gelatin in water and adding suflicient alkali to give a pH of above 7.5, preferably between 8 and 9 (Solution 1). Separate solutions are then made up from water, silver (Solution 1) and from water, sodium sulfite and tannic acid (Solution III).
- Solution II is added to Solution I and after a pause of 2 to 5,:Solution III is dumped inwith vigorous agitation, preferably while using several stirrers.
- the emulsion is digested at 40 C., for about 20 minutes, chilled, shredded and Washed. Alternatively, the dispersion may be coagulated, washed, remelted and chilled.
- the quantities of the various essential components may vary so long as there is present, the aforesaid minimum of strontium nitrate and an adequate quantity of silver salt and reducing agent to yield the dense blue colored dispersion.
- I may employ .2 to .4 kilo of silver nitrate, .015 to .10 kilo of strontium nitrate, .1 to .4 kilo of sodium sulfite and .2 to .4 kilo of tannic acid.
- the proportions of the ingredients used in the above patent US. 2,688,601 are adequate.
- the resulting dispersion is coated on a film support in the usual manner and dried to produce a very effective bluev colored antihalation layer- When coated at a concentration of 3.2 milligrams of silver per 100 square centimeters, the optical density is 0.15 at 450 my and 2.35 at 650 ma. 7
- I claim; 7 -1 A method ofpreparing a blue color dispersion of silver in gelatin comprising admixing an aqueous alkaline gelatin solution with a water soluble silver salt and at least about .005 mol'of a water soluble strontium salt per liter of the reaction mixture, and eflecting reduction of the silver salt by adding an amount of an alkali metal sulfite which is at least one half of the weight of the silver salt and an excess of tannic acid.
- a stable dispersion of silver in gelatin said dispersion having a dense 'blue color and being particularly adapted for use as an anti-halation layer for a multilayer color film, said dispersion being prepared according to the procedure of, claim 1.
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Colloid Chemistry (AREA)
- Heterocyclic Carbon Compounds Containing A Hetero Ring Having Nitrogen And Oxygen As The Only Ring Hetero Atoms (AREA)
- Pyridine Compounds (AREA)
Priority Applications (4)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
BE562967D BE562967A (en, 2012) | 1957-02-13 | ||
US639863A US2921914A (en) | 1957-02-13 | 1957-02-13 | Preparation of blue colloidal silver dispersions for antihalo layer |
DEG23698A DE1075942B (de) | 1957-02-13 | 1958-01-10 | Verfahren zur Herstellung einer blaugefaerbten Dispersion von kolloidalem Silber fuer Lichthofschutzschichten |
GB2714/58A GB843713A (en) | 1957-02-13 | 1958-01-27 | Preparation of blue colloidal silver dispersions for photographic antihalo layers |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US639863A US2921914A (en) | 1957-02-13 | 1957-02-13 | Preparation of blue colloidal silver dispersions for antihalo layer |
Publications (1)
Publication Number | Publication Date |
---|---|
US2921914A true US2921914A (en) | 1960-01-19 |
Family
ID=24565873
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
US639863A Expired - Lifetime US2921914A (en) | 1957-02-13 | 1957-02-13 | Preparation of blue colloidal silver dispersions for antihalo layer |
Country Status (4)
Country | Link |
---|---|
US (1) | US2921914A (en, 2012) |
BE (1) | BE562967A (en, 2012) |
DE (1) | DE1075942B (en, 2012) |
GB (1) | GB843713A (en, 2012) |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3655412A (en) * | 1967-11-15 | 1972-04-11 | Fuji Photo Film Co Ltd | Process for the production of dispersions of colloidal silver |
US4563406A (en) * | 1981-10-07 | 1986-01-07 | Konishiroku Photo Industry Co., Ltd. | Light-sensitive silver halide photographic material with white layer and colorant containing layer |
US5246823A (en) * | 1991-05-14 | 1993-09-21 | Eastman Kodak Company | Photographic element having improved antihalation layer containing tabular silver grains |
US5753402A (en) * | 1995-07-31 | 1998-05-19 | Eastman Kodak Company | Method for recording and processing motion picture film soundtrack |
Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US2688601A (en) * | 1951-09-27 | 1954-09-07 | Eastman Kodak Co | Preparation of silver dispersions |
-
0
- BE BE562967D patent/BE562967A/xx unknown
-
1957
- 1957-02-13 US US639863A patent/US2921914A/en not_active Expired - Lifetime
-
1958
- 1958-01-10 DE DEG23698A patent/DE1075942B/de active Pending
- 1958-01-27 GB GB2714/58A patent/GB843713A/en not_active Expired
Patent Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US2688601A (en) * | 1951-09-27 | 1954-09-07 | Eastman Kodak Co | Preparation of silver dispersions |
Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3655412A (en) * | 1967-11-15 | 1972-04-11 | Fuji Photo Film Co Ltd | Process for the production of dispersions of colloidal silver |
US4563406A (en) * | 1981-10-07 | 1986-01-07 | Konishiroku Photo Industry Co., Ltd. | Light-sensitive silver halide photographic material with white layer and colorant containing layer |
US5246823A (en) * | 1991-05-14 | 1993-09-21 | Eastman Kodak Company | Photographic element having improved antihalation layer containing tabular silver grains |
US5318885A (en) * | 1991-05-14 | 1994-06-07 | Eastman Kodak Company | Photographic element having improved antihalation layer |
US5753402A (en) * | 1995-07-31 | 1998-05-19 | Eastman Kodak Company | Method for recording and processing motion picture film soundtrack |
Also Published As
Publication number | Publication date |
---|---|
DE1075942B (de) | 1960-02-18 |
GB843713A (en) | 1960-08-10 |
BE562967A (en, 2012) |
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