US2618556A - Process for preparing photographic emulsions - Google Patents
Process for preparing photographic emulsions Download PDFInfo
- Publication number
- US2618556A US2618556A US787028A US78702847A US2618556A US 2618556 A US2618556 A US 2618556A US 787028 A US787028 A US 787028A US 78702847 A US78702847 A US 78702847A US 2618556 A US2618556 A US 2618556A
- Authority
- US
- United States
- Prior art keywords
- water
- emulsion
- silver
- soluble
- halide
- 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
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- 239000000839 emulsion Substances 0.000 title claims description 103
- 238000004519 manufacturing process Methods 0.000 title claims description 19
- 229910052709 silver Inorganic materials 0.000 claims description 74
- 239000004332 silver Substances 0.000 claims description 74
- -1 SILVER HALIDE Chemical class 0.000 claims description 73
- 150000003839 salts Chemical class 0.000 claims description 46
- 229920000159 gelatin Polymers 0.000 claims description 33
- 235000019322 gelatine Nutrition 0.000 claims description 32
- 239000008273 gelatin Substances 0.000 claims description 30
- 108010010803 Gelatin Proteins 0.000 claims description 29
- 235000011852 gelatine desserts Nutrition 0.000 claims description 29
- 239000006228 supernatant Substances 0.000 claims description 29
- 239000000203 mixture Substances 0.000 claims description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 26
- 150000004820 halides Chemical class 0.000 claims description 23
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 18
- 239000002253 acid Substances 0.000 claims description 16
- 230000029087 digestion Effects 0.000 claims description 14
- 230000015572 biosynthetic process Effects 0.000 claims description 13
- 229910052783 alkali metal Inorganic materials 0.000 claims description 8
- 150000001340 alkali metals Chemical class 0.000 claims description 8
- 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 8
- 229910052751 metal Inorganic materials 0.000 claims description 6
- 239000002184 metal Substances 0.000 claims description 6
- 150000002739 metals Chemical class 0.000 claims description 6
- 150000003863 ammonium salts Chemical class 0.000 claims description 5
- 229910017053 inorganic salt Inorganic materials 0.000 claims description 5
- 230000000737 periodic effect Effects 0.000 claims description 5
- 238000000034 method Methods 0.000 description 22
- 239000000243 solution Substances 0.000 description 18
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 16
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 14
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 12
- 238000005406 washing Methods 0.000 description 11
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 10
- 229910001961 silver nitrate Inorganic materials 0.000 description 8
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 6
- 239000011780 sodium chloride Substances 0.000 description 6
- 229910001508 alkali metal halide Inorganic materials 0.000 description 5
- 150000008045 alkali metal halides Chemical class 0.000 description 5
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 5
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 5
- 235000011130 ammonium sulphate Nutrition 0.000 description 5
- 230000001112 coagulating effect Effects 0.000 description 5
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- 239000001828 Gelatine Substances 0.000 description 3
- 150000001768 cations Chemical class 0.000 description 3
- 230000015271 coagulation Effects 0.000 description 3
- 238000005345 coagulation Methods 0.000 description 3
- 238000010908 decantation Methods 0.000 description 3
- 239000000499 gel Substances 0.000 description 3
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical compound [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- CPELXLSAUQHCOX-UHFFFAOYSA-M Bromide Chemical compound [Br-] CPELXLSAUQHCOX-UHFFFAOYSA-M 0.000 description 2
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 2
- 150000007513 acids Chemical class 0.000 description 2
- ZCCIPPOKBCJFDN-UHFFFAOYSA-N calcium nitrate Chemical compound [Ca+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ZCCIPPOKBCJFDN-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 235000019441 ethanol Nutrition 0.000 description 2
- 239000008394 flocculating agent Substances 0.000 description 2
- 238000001879 gelation Methods 0.000 description 2
- IOLCXVTUBQKXJR-UHFFFAOYSA-M potassium bromide Chemical compound [K+].[Br-] IOLCXVTUBQKXJR-UHFFFAOYSA-M 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- ZSLUVFAKFWKJRC-IGMARMGPSA-N 232Th Chemical compound [232Th] ZSLUVFAKFWKJRC-IGMARMGPSA-N 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 229910021607 Silver chloride Inorganic materials 0.000 description 1
- 229910052776 Thorium Inorganic materials 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- SJOOOZPMQAWAOP-UHFFFAOYSA-N [Ag].BrCl Chemical compound [Ag].BrCl SJOOOZPMQAWAOP-UHFFFAOYSA-N 0.000 description 1
- HOLVRJRSWZOAJU-UHFFFAOYSA-N [Ag].ICl Chemical compound [Ag].ICl HOLVRJRSWZOAJU-UHFFFAOYSA-N 0.000 description 1
- 150000001242 acetic acid derivatives Chemical class 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 239000011609 ammonium molybdate Substances 0.000 description 1
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 description 1
- 235000018660 ammonium molybdate Nutrition 0.000 description 1
- 229940010552 ammonium molybdate Drugs 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- OIDPCXKPHYRNKH-UHFFFAOYSA-J chrome alum Chemical compound [K]OS(=O)(=O)O[Cr]1OS(=O)(=O)O1 OIDPCXKPHYRNKH-UHFFFAOYSA-J 0.000 description 1
- 239000000701 coagulant Substances 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 235000015110 jellies Nutrition 0.000 description 1
- 239000008274 jelly Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 150000002823 nitrates Chemical class 0.000 description 1
- 235000021317 phosphate Nutrition 0.000 description 1
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000009877 rendering Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- ADZWSOLPGZMUMY-UHFFFAOYSA-M silver bromide Chemical compound [Ag]Br ADZWSOLPGZMUMY-UHFFFAOYSA-M 0.000 description 1
- ZUNKMNLKJXRCDM-UHFFFAOYSA-N silver bromoiodide Chemical compound [Ag].IBr ZUNKMNLKJXRCDM-UHFFFAOYSA-N 0.000 description 1
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 description 1
- 229960001763 zinc sulfate Drugs 0.000 description 1
- 229910000368 zinc sulfate Inorganic materials 0.000 description 1
- 229910052726 zirconium Inorganic materials 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
- G03C1/005—Silver halide emulsions; Preparation thereof; Physical treatment thereof; Incorporation of additives therein
- G03C1/015—Apparatus or processes for the preparation of emulsions
Definitions
- Washed gelatino-silver-halide 5 tains the Water-soluble salts generated during photographic emulsions have been prepared by the formation of the silver halide emulsion from a process consisting of the following general a water-soluble silver salt and a water-soluble steps: halide, a water-soluble salt selected from the (1) Preparation of a silver halide in a watergroup consisting of ammonium salts, salts of the solution of gelatin by mixing a water-solution of alkali metals having an atomic weight less than a water-soluble silver salt (usually silver nitrate) 140, and salts of metals of group II of the periwith a water solution of a water-soluble halide odic arrangement of elements having an atomic (usually an ammonium halide or a halide of an weight of less than 140, in quantity sufficient to alkali metal).
- halide a water-soluble salt selected from the (1) Preparation of a silver halide in a watergroup consist
- the gelatin may be dissolved in coagulate the silver halide, and also add to the either or both of these solutions, or in a separate emulsion a water-soluble acid capable of lowersolu-tion. ing the pH of the emulsion to at least 4, in quan- (2) After the silver halide has been formed, tity sufiicient to lower the pH of the emulsion the emulsion is digested, to a greater or lesser to at least 6, whereupon the silver halide settles extent, in the presence or absence of other chemout rapidly and can be readily separated from the icals, to produce the desired grain size, grain size 1iquid portion of the mixture, washed and redisdistribution, and grain sensitivity.
- the process can be (3) The emulsion is then chilled and allowed carried out at any convenient temperature, to gel. More gelatin may be added before chilladvantageously from '75 to 110 F., in the case of ing, if necessary to raise the gelatin concentragelatino-silver-halide emulsions.
- the salt or the tion so that the emulsion may be set to form acid may be added to the emulsion first or the a jelly. salt and acid can be added simultaneously.
- the collold can be d1Ss1Ved 1n elther digestion at more or less elevated temperatures.
- Our process differs from the aforesaid process in that it is carried out at a pH of 6 or lower, and the ammonium salts and the salts of the alkali metals and the salts of metals of group 11 of the periodic table having an atomic weight of less than 140, coagulate the silver halide itself rather than the gelatin, although when operating our process at a pH near the isoelectric point of the gelatin in a gelatino-silver-halide emulsion some of the gelatin is coagulated but not permanently hardened.
- This washing process was repeated three times, each time adding enough water to make the total volume up to about twice the original volume of uncoagulated emulsion. After the final decantation, enough water was added to make the volume up to a volume equaling the original emulsion volume.
- the total bulk was then made up to 12,500 grams with water and the resulting emulsion digested (ripened) in the usual manner.
- Example 2 An emulsion was prepared exactly as in Example 1, except that hydrochloric acid instead of sulfuric acid was employed to lower the pH of the emulsion to at least 3.
- Example 3 An emulsion was prepared exactly as in Example 1, except that hydrochloric acid was employed instead of sulfuric acid to lower the pH of the emulsion to at least 3 and 650 grams of zinc sulfate was employed instead of sodium chloride to coagulate the silver halide.
- Example 4 An emulsion was prepared exactly as in Example 1, except that after the decantation of the supernatant liquor from the first settling operation, 50 grams of dry sodium sulfate (anhydrous) was added. This addition helps to prevent resuspension of the silver halide grains during subsequent washing.
- Example 5 An emulsion was prepared exactly as in Example 1, except that 500 grams of ammonium sulfate was employed instead of sodium chloride to coagulate the silver halide.
- Example 6 Ammonium bromide Ammonium chloride Ammonium phosphate Ammonium sulfate Ammonium molybdate Ammonium nitrate Barium chloride Barium nitrate Calcium chloride Calcium nitrate Magnesium sulfate" Potassium persulfate Potassium ferrocyanide Potassium ferricyanide Potassium sulfate Potassium chromate Potassium chloride Sodium sulfate Sodium chloride Sodium tetraborate Sodium acetate Trisodium phosphate Zinc chloride Zinc sulfate Zinc nitrate Zinc bromide Saltscontaining monovalent cations are advantageously employed. One or more salts can be employed.
- the salt can'be added to the emulsion before the pH is lowered'by the addition of the acids. More or less digestion time may be given before adding the acid and salt to effect coagulation. Additional gelatin can be added before the coagulation, if desired. Temperatures varied within wide limits and depend more upon the emulsion characteristics desired than upon the requirements of the process. More or less washing of the coagulated silver halide grains may be employed, again depending upon the emulsion characteristics desired. Also the quantitles of acids and salts employed may vary within Wide limits; the optimum quantities being readily determined for each individual emulsion by making simple observations.
- the quantity of acid used to lower the pH of the emulsion can be varied within relatively wide limits.
- the actual pH value to be obtained depends not only upon the particular coagulating salt which is employed but also upon the quantity of the coagulating salt.
- the optimum quantity of acid will correspond to the quantity at which the minimum amount of coagulating salt is required.
- the kind :of acid employed also has some effect upon the amount required and upon the optimum value of pH.
- the quantity of coagulating salts can be varied within wide limits. Some salts, particularly nitrates and acetates, must be employed in relatively large quantities.
- Li l Others notably sulfates, phosphates, and molybdatesv may be used in relatively small quantities. It appears that the anion in any given salt is more important in determining the effectiveness of the salt than is the cation.
- Some salts for example, ammonium molybdate, can be used in amounts as low as one part per .500 parts of photographic emulsion, by weight. Others, e. g. calcium nitrate must be employed at the rate of 1 part per 5 parts of emulsion.
- the entire making, washing and finishing operations ordinarily employed in emulsion making may be carried out in one container, one operation following immediately after'th'e preceding one without delay forchilling, washing'and draining.
- any of the customarily employed washed emulsions can be prepared by our new process, e. g. silver bromide, silver bromoiodide, silver chlorobromide, silver chlorobromoiodide, silver chloride, silver chloroiodide, etc. emulsions.
- th steps which consist in (1) adding to a gelatino-silver-halide emulsion which contains the water-soluble salts generated during the formation of the silver halide from a water-soluble silver salt and a water-soluble halide, after completion of the first digestion, at least one water-soluble, inorganic salt selected from the group consisting of ammonium salts, salts of the alkali metals having an atomic weight less than 1-10 and salts of metals of group II of the periodic arrangement of elements having an atomic weight less than 140,
- a gelatino-silver-halide emulsion which contains the water-soluble salts generated during the formation of the silver halide from a water-soluble silver salt and a water-soluble halide, after completionof theflrst digestion, sodium chloride, in quantity sufiicient to coagulate the silver halide, and also adding to the emulsion hydrochloric acid in quantity sufficient to lower the pI-I of the emulsion to at least 6, (2) decanting the supernatant liquor, (3) adding water to the coagulated, substantially gelatin-free silver halide, (4) agitating the mixture thus obtained, settling the mixture, (6) decanting the supernatant liquor, said steps (2), (3), (4), (5) and (6) being performed successively until the concentration of the Watersoluble halides is reduced to the desired level, and (7) redispersing the washe
- a process for preparing a photographic gelatino-silver-halide emulsion the steps which consist in (1) adding to a gelatino-silver-halide emulsion which contains the water-soluble salts generated during the formation of the silver halide from a water-soluble silver salt and a water-soluble halide, after completion of the first digestion, ammonium sulfate, in quantity sufficient to coagulate the silver halide, and also adding to the emulsion sulfuric acid and citric acid in quantity sufficient to lower the pH of the emulsion to at least 6, (2) decanting the supernatant liquor, (3) adding water to the coagulated, substantially gelatin-free silver halide, (4) agitating the mixture thus obtained, (5) settling the mixture, (6) decanting the supernatant liquor, said steps (2), (3), (4), (5) and (6) being performed successively until the concentration of the water-soluble halides is reduced to the desired level, and (7) redispersing the washed silver
- a gelatino-silver-halide emulsion which contains the water-soluble salts generated during the formation of the silver halide from a water-soluble silver salt and a water-soluble halide, after completion of the first digestion, an inorganic salt of an alkali metal having an atomic weight less than 140, in quantity sufficient to coagulate the silver halide, and also adding to the emulsion a water-soluble acid having an ionization constant at least that of acetic acid in quantity sumcient to lower the pH of the emulsion to at least 6, (2) decanting the supernatant liquor, (3) adding water to the coagulated, substantially gelatin-free silver halide,
- a process for preparing a photographic gelatino-silver-halide emulsion the steps which consist in (1) adding to a gelatino-silver-halide emulsion which contains the water-soluble salts generated during the formation of the silver halide from a water-soluble salt and a watersoluble halide, after completion of the first digestion, an inorganic ammonium (NH4) salt in quantity sufficient to coagulate the silver halide, and also adding to the emulsion a water-soluble acid having an ionization constant at least that of acetic acid in quantity sufficient to lower the pH of the emulsion to at least 6, (2) decanting the supernatant liquor, (3) adding water to the coagulated, substantially gelatin-free silver halide, (4) agitating the mixturethus obtained, (5) settling the mixture, (6) decanting the supernatant liquor, said steps (2), (3), (4), (5) and (6) being performed successively until the concentration of the water-soluble halides is reduced to the
- a process for preparing a photographic gelatino-silver-halide emulsion the steps which consist in (1) adding to a gelatino-silver-halide emulsion which contains the water-soluble salts generated during the formation of the silver halide from silver nitrate and an alkali metal halide, after completion of the first digestion, at least one Water-soluble, inorganic salt selected from the group consisting of ammonium salts, salts of the alkali metals having an atomic weight less than and salts of metals of group II of the periodic arrangement of elements having an atomic weight less than 140, in quantity sufiicient to coagulate the silver halide, and also adding to the emulsion at least one water-soluble acid having an ionization constant at least that of acetic acid in quantity sufficient to lower the pH to at least 6, (2) decanting the supernatant liquor, (3) adding water to the coagulated, substantially gelatin-free silver halide, (4) agitating the mixture thus obtained,
- a gelatino-silver-halide emulsion which contains the water-soluble salts generated during the formation of the silver halide from silver nitrate and an alkali metal halide, after completion of the first digestion, an inorganic salt of an alkali metal having an atomic weight less than 140, in quantity sufficient to coagulate the silver halide, and also adding to the emulsion a water-soluble acid having an ionization constant at least that of acetic acid in quantity sufiicient to lower the pH of the emulsion to at least 6, (2) decantin the supernatant liquor, (3) adding water to the coagulated, substantially gelatin-free silver halide, (4) agitating the mixture thus obtained, (5) settling the mixture, (6) decanting the supernatant liquor, said steps (2), (3), (4), (5) and (6) being performed successively until the
- a process for preparing a photographic gelatino-silver-halide emulsion the steps which consists in 1) adding to a gelatino-silver-halide emulsion which contains the water-soluble salts generated during the formation of the silver halide from silver nitrate and an alkali metal halide, after completion of the first digestion, ammonium sulfate in quantity suflicient to coagulate the silver halide, and also adding to the emulsion sulfuric acid and citric acid in quantity sufficient to lower the pH of the emulsion to at least 6, (2) decanting the supernatant liquor, (3) adding water to the coagulated, substantially gelatin-free silver halide (4) agitating the mixture thus obtained, (5) settling the mixture, (6) decanting the supernatant liquor, said steps (2), (3), (4), (5) and (6) being performed successively until the concentration of the water-soluble halides is reduced to the desired level, and (7 redispersing the washed silver
- a process for preparing a photographic gelatino-silver-halide emulsion the steps which consist in (1) adding to a gelatino-silver-halide emulsion which contains the water-soluble salts generated during the formation of the silver halide from silver nitrate and an alkali metal halide, after completion of the first digestion, ammonium sulfate in quantity sufficient to coagulate the silver halide, and also adding to the emulsion sulfuric acid in quantity sufficient to lower the pH of the emulsion to at least 6, (2) decanting the supernatant liquor, (3) adding water to the coagulated, substantially gelatin-free silver halide, (4) agitating the mixture thus obtained, (5) settling the mixture, (6) decanting the supernatant liquor, said steps (2), .(3), (4), (5) and (6) being performed successively until the concentration of the water-soluble halides is reduced to the desired level, and (7 redispersing the washed silver halide grains in an
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Colloid Chemistry (AREA)
Priority Applications (4)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| BE484329D BE484329A (en)) | 1947-11-19 | ||
| US787028A US2618556A (en) | 1947-11-19 | 1947-11-19 | Process for preparing photographic emulsions |
| GB5490/48A GB655082A (en) | 1947-11-19 | 1948-02-24 | Improvements in the production of photographic emulsions |
| FR980385D FR980385A (fr) | 1947-11-19 | 1948-08-10 | Procédé perfectionné de préparation d'émulsions de gélatino-halogénures d'argent et produits en résultant |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US787028A US2618556A (en) | 1947-11-19 | 1947-11-19 | Process for preparing photographic emulsions |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| US2618556A true US2618556A (en) | 1952-11-18 |
Family
ID=25140222
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| US787028A Expired - Lifetime US2618556A (en) | 1947-11-19 | 1947-11-19 | Process for preparing photographic emulsions |
Country Status (4)
| Country | Link |
|---|---|
| US (1) | US2618556A (en)) |
| BE (1) | BE484329A (en)) |
| FR (1) | FR980385A (en)) |
| GB (1) | GB655082A (en)) |
Cited By (45)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2768079A (en) * | 1954-01-25 | 1956-10-23 | Eastman Kodak Co | Method of preparing washed photographic emulsions |
| US2816029A (en) * | 1955-03-08 | 1957-12-10 | Eastman Kodak Co | Supersensitizing combinations comprising simple cyanine dyes and metal salts |
| US2819964A (en) * | 1955-03-08 | 1958-01-14 | Eastman Kodak Co | Supersensitizing combinations comprising meso-substituted carbocyanine dyes and metal salts |
| US2839405A (en) * | 1955-03-08 | 1958-06-17 | Eastman Kodak Co | Inorganic salt antifoggants for photographic emulsions |
| US2843490A (en) * | 1955-03-08 | 1958-07-15 | Eastman Kodak Co | Supersensitizing combinations comprising meso-substituted carbocyanine dyes and polyvalent metal salts |
| US2950972A (en) * | 1954-11-24 | 1960-08-30 | Gen Aniline & Film Corp | Photographic emulsions having increased sensitivity to x-ray and gamma ray radiation |
| US3000739A (en) * | 1957-04-02 | 1961-09-19 | Du Pont | Process for preparing silver halide emulsions |
| US3007796A (en) * | 1959-02-25 | 1961-11-07 | Gen Foods Corp | Process for preparing photographic emulsions |
| US3031304A (en) * | 1958-08-20 | 1962-04-24 | Albert J Oliver | Fine grain nuclear emulsion |
| US3088824A (en) * | 1959-02-17 | 1963-05-07 | Cons Electrodynamics Corp | Rapid photographic developing |
| US3144335A (en) * | 1961-03-06 | 1964-08-11 | Polaroid Corp | Process for producing silver halidecasein photographic emulsions |
| US3153593A (en) * | 1961-05-08 | 1964-10-20 | Gevaert Photo Prod Nv | Manufacture of silver halide emulsions |
| US3153594A (en) * | 1959-07-07 | 1964-10-20 | Du Pont | Process for preparing photographic emulsions |
| US3201250A (en) * | 1959-01-12 | 1965-08-17 | Eastman Kodak Co | Dimensionally stable gelatincontaining film product |
| US3236653A (en) * | 1958-03-20 | 1966-02-22 | Gevaert Photo Prod Nv | Hardening of polyvinyl alcohol maleates |
| US3260605A (en) * | 1962-01-05 | 1966-07-12 | Eastman Kodak Co | Method for preparing light-sensitive silver halide emulsions suitable for print-out recording materials |
| US3260598A (en) * | 1961-05-29 | 1966-07-12 | Eastman Kodak Co | Photographic element-developer system |
| US3272631A (en) * | 1964-01-03 | 1966-09-13 | Du Pont | Haze reduction of photographic emulsions containing a covering power agent |
| US3628959A (en) * | 1967-10-23 | 1971-12-21 | Horst Theilemann | Process for the preparation of photographic emulsion |
| US3784381A (en) * | 1970-11-13 | 1974-01-08 | Eastman Kodak Co | High speed silver chloroiodide emulsions |
| US3847616A (en) * | 1971-02-08 | 1974-11-12 | Fuji Photo Film Co Ltd | Process and apparatus for gelling a sol-form substance for a photographic light-sensitive element and for melting same |
| EP0115351A2 (en) | 1983-01-28 | 1984-08-08 | Fuji Photo Film Co., Ltd. | Silver halide light-sensitive material |
| US4681838A (en) * | 1984-06-15 | 1987-07-21 | Fuji Photo Film Co., Ltd. | Silver halide photographic emulsion and process for production thereof |
| US4863845A (en) * | 1984-06-15 | 1989-09-05 | Fuji Photo Film Co., Ltd. | Internal latent image type direct positive silver halide emulsions and process for producing the same |
| US4925783A (en) * | 1987-05-15 | 1990-05-15 | Konica Corporation | High sensitivity light-sensitive silver halide photographic material with little stain |
| EP0691569A1 (en) | 1994-07-04 | 1996-01-10 | Kodak-Pathe | Photographic emulsion with improved sensitivity |
| US5492805A (en) * | 1994-06-30 | 1996-02-20 | Minnesota Mining And Manufacturing Company | Blocked leuco dyes for photothermographic elements |
| US5492804A (en) * | 1994-06-30 | 1996-02-20 | Minnesota Mining And Manufacturing Company | Chromogenic leuco redox-dye-releasing compounds for photothermographic elements |
| US5492803A (en) * | 1995-01-06 | 1996-02-20 | Minnesota Mining And Manufacturing Company | Hydrazide redox-dye-releasing compounds for photothermographic elements |
| US5891615A (en) * | 1997-04-08 | 1999-04-06 | Imation Corp. | Chemical sensitization of photothermographic silver halide emulsions |
| US5928857A (en) * | 1994-11-16 | 1999-07-27 | Minnesota Mining And Manufacturing Company | Photothermographic element with improved adherence between layers |
| US5939249A (en) * | 1997-06-24 | 1999-08-17 | Imation Corp. | Photothermographic element with iridium and copper doped silver halide grains |
| US5972591A (en) * | 1990-12-20 | 1999-10-26 | Eastman Kodak Company | Thickener for delivery of photographic emulsions |
| US5994049A (en) * | 1997-08-28 | 1999-11-30 | Eastman Kodak Company | Water-soluble non-interactive polymers and surfactant micelles for desalting and concentrating silver halide photographic emulsions |
| US6004740A (en) * | 1997-08-28 | 1999-12-21 | Eastman Kodak Company | Water-soluble non-interactive carboxyl polymers for desalting and concentrating silver halide photographic emulsions |
| US6117624A (en) * | 1993-06-04 | 2000-09-12 | Eastman Kodak Company | Infrared sensitized, photothermographic article |
| US6171707B1 (en) | 1994-01-18 | 2001-01-09 | 3M Innovative Properties Company | Polymeric film base having a coating layer of organic solvent based polymer with a fluorinated antistatic agent |
| US7468241B1 (en) | 2007-09-21 | 2008-12-23 | Carestream Health, Inc. | Processing latitude stabilizers for photothermographic materials |
| US7524621B2 (en) | 2007-09-21 | 2009-04-28 | Carestream Health, Inc. | Method of preparing silver carboxylate soaps |
| US7622247B2 (en) | 2008-01-14 | 2009-11-24 | Carestream Health, Inc. | Protective overcoats for thermally developable materials |
| CN101256346B (zh) * | 2008-02-04 | 2010-09-29 | 黄山银江科技有限公司 | 一种激光照排胶片的生产方法 |
| WO2015148028A1 (en) | 2014-03-24 | 2015-10-01 | Carestream Health, Inc. | Thermally developable imaging materials |
| WO2016073086A1 (en) | 2014-11-04 | 2016-05-12 | Carestream Health, Inc. | Image forming materials, preparations, and compositions |
| WO2016195950A1 (en) | 2015-06-02 | 2016-12-08 | Carestream Health, Inc. | Thermally developable imaging materials and methods |
| WO2017123444A1 (en) | 2016-01-15 | 2017-07-20 | Carestream Health, Inc. | Method of preparing silver carboxylate soaps |
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| US1844716A (en) * | 1929-04-19 | 1932-02-09 | Eastman Kodak Co | Process of making photographic emulsions |
| US2258755A (en) * | 1938-06-23 | 1941-10-14 | Chromogen Inc | Process for the manufacture of dyed gelatin layers for photographic purposes |
| US2401051A (en) * | 1939-09-26 | 1946-05-28 | Photo Positive Corp | Photographic emulsions and methods |
| GB585758A (en) * | 1944-10-30 | 1947-02-24 | John Alfred Henry Hart | Improvements in or relating to the production of photographic emulsions |
| US2489341A (en) * | 1944-07-04 | 1949-11-29 | Ilford Ltd | Production of photographic silver halide emulsions |
-
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- 1948-08-10 FR FR980385D patent/FR980385A/fr not_active Expired
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US1844716A (en) * | 1929-04-19 | 1932-02-09 | Eastman Kodak Co | Process of making photographic emulsions |
| US2258755A (en) * | 1938-06-23 | 1941-10-14 | Chromogen Inc | Process for the manufacture of dyed gelatin layers for photographic purposes |
| US2401051A (en) * | 1939-09-26 | 1946-05-28 | Photo Positive Corp | Photographic emulsions and methods |
| US2489341A (en) * | 1944-07-04 | 1949-11-29 | Ilford Ltd | Production of photographic silver halide emulsions |
| GB585758A (en) * | 1944-10-30 | 1947-02-24 | John Alfred Henry Hart | Improvements in or relating to the production of photographic emulsions |
Cited By (51)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2768079A (en) * | 1954-01-25 | 1956-10-23 | Eastman Kodak Co | Method of preparing washed photographic emulsions |
| US2950972A (en) * | 1954-11-24 | 1960-08-30 | Gen Aniline & Film Corp | Photographic emulsions having increased sensitivity to x-ray and gamma ray radiation |
| US2816029A (en) * | 1955-03-08 | 1957-12-10 | Eastman Kodak Co | Supersensitizing combinations comprising simple cyanine dyes and metal salts |
| US2819964A (en) * | 1955-03-08 | 1958-01-14 | Eastman Kodak Co | Supersensitizing combinations comprising meso-substituted carbocyanine dyes and metal salts |
| US2839405A (en) * | 1955-03-08 | 1958-06-17 | Eastman Kodak Co | Inorganic salt antifoggants for photographic emulsions |
| US2843490A (en) * | 1955-03-08 | 1958-07-15 | Eastman Kodak Co | Supersensitizing combinations comprising meso-substituted carbocyanine dyes and polyvalent metal salts |
| US3000739A (en) * | 1957-04-02 | 1961-09-19 | Du Pont | Process for preparing silver halide emulsions |
| US3236653A (en) * | 1958-03-20 | 1966-02-22 | Gevaert Photo Prod Nv | Hardening of polyvinyl alcohol maleates |
| US3031304A (en) * | 1958-08-20 | 1962-04-24 | Albert J Oliver | Fine grain nuclear emulsion |
| US3201250A (en) * | 1959-01-12 | 1965-08-17 | Eastman Kodak Co | Dimensionally stable gelatincontaining film product |
| US3088824A (en) * | 1959-02-17 | 1963-05-07 | Cons Electrodynamics Corp | Rapid photographic developing |
| US3007796A (en) * | 1959-02-25 | 1961-11-07 | Gen Foods Corp | Process for preparing photographic emulsions |
| US3153594A (en) * | 1959-07-07 | 1964-10-20 | Du Pont | Process for preparing photographic emulsions |
| US3144335A (en) * | 1961-03-06 | 1964-08-11 | Polaroid Corp | Process for producing silver halidecasein photographic emulsions |
| US3153593A (en) * | 1961-05-08 | 1964-10-20 | Gevaert Photo Prod Nv | Manufacture of silver halide emulsions |
| US3260598A (en) * | 1961-05-29 | 1966-07-12 | Eastman Kodak Co | Photographic element-developer system |
| US3260605A (en) * | 1962-01-05 | 1966-07-12 | Eastman Kodak Co | Method for preparing light-sensitive silver halide emulsions suitable for print-out recording materials |
| US3272631A (en) * | 1964-01-03 | 1966-09-13 | Du Pont | Haze reduction of photographic emulsions containing a covering power agent |
| US3628959A (en) * | 1967-10-23 | 1971-12-21 | Horst Theilemann | Process for the preparation of photographic emulsion |
| US3784381A (en) * | 1970-11-13 | 1974-01-08 | Eastman Kodak Co | High speed silver chloroiodide emulsions |
| US3847616A (en) * | 1971-02-08 | 1974-11-12 | Fuji Photo Film Co Ltd | Process and apparatus for gelling a sol-form substance for a photographic light-sensitive element and for melting same |
| EP0115351A2 (en) | 1983-01-28 | 1984-08-08 | Fuji Photo Film Co., Ltd. | Silver halide light-sensitive material |
| US4681838A (en) * | 1984-06-15 | 1987-07-21 | Fuji Photo Film Co., Ltd. | Silver halide photographic emulsion and process for production thereof |
| US4863845A (en) * | 1984-06-15 | 1989-09-05 | Fuji Photo Film Co., Ltd. | Internal latent image type direct positive silver halide emulsions and process for producing the same |
| US4925783A (en) * | 1987-05-15 | 1990-05-15 | Konica Corporation | High sensitivity light-sensitive silver halide photographic material with little stain |
| US5972591A (en) * | 1990-12-20 | 1999-10-26 | Eastman Kodak Company | Thickener for delivery of photographic emulsions |
| US6117624A (en) * | 1993-06-04 | 2000-09-12 | Eastman Kodak Company | Infrared sensitized, photothermographic article |
| US6171707B1 (en) | 1994-01-18 | 2001-01-09 | 3M Innovative Properties Company | Polymeric film base having a coating layer of organic solvent based polymer with a fluorinated antistatic agent |
| US5492805A (en) * | 1994-06-30 | 1996-02-20 | Minnesota Mining And Manufacturing Company | Blocked leuco dyes for photothermographic elements |
| US5492804A (en) * | 1994-06-30 | 1996-02-20 | Minnesota Mining And Manufacturing Company | Chromogenic leuco redox-dye-releasing compounds for photothermographic elements |
| US5696289A (en) * | 1994-06-30 | 1997-12-09 | Minnesota Mining And Manufacturing Company | Blocked leuco dyes for photothermographic elements |
| US5705676A (en) * | 1994-06-30 | 1998-01-06 | Minnesota Mining And Manufacturing Company | Chromogenic leuco redox-dye-releasing compounds for photothermographic elements |
| EP0691569A1 (en) | 1994-07-04 | 1996-01-10 | Kodak-Pathe | Photographic emulsion with improved sensitivity |
| US5928857A (en) * | 1994-11-16 | 1999-07-27 | Minnesota Mining And Manufacturing Company | Photothermographic element with improved adherence between layers |
| US5492803A (en) * | 1995-01-06 | 1996-02-20 | Minnesota Mining And Manufacturing Company | Hydrazide redox-dye-releasing compounds for photothermographic elements |
| US5891615A (en) * | 1997-04-08 | 1999-04-06 | Imation Corp. | Chemical sensitization of photothermographic silver halide emulsions |
| US6060231A (en) * | 1997-06-24 | 2000-05-09 | Eastman Kodak Company | Photothermographic element with iridium and copper doped silver halide grains |
| US5939249A (en) * | 1997-06-24 | 1999-08-17 | Imation Corp. | Photothermographic element with iridium and copper doped silver halide grains |
| US6004740A (en) * | 1997-08-28 | 1999-12-21 | Eastman Kodak Company | Water-soluble non-interactive carboxyl polymers for desalting and concentrating silver halide photographic emulsions |
| US5994049A (en) * | 1997-08-28 | 1999-11-30 | Eastman Kodak Company | Water-soluble non-interactive polymers and surfactant micelles for desalting and concentrating silver halide photographic emulsions |
| US7468241B1 (en) | 2007-09-21 | 2008-12-23 | Carestream Health, Inc. | Processing latitude stabilizers for photothermographic materials |
| US7524621B2 (en) | 2007-09-21 | 2009-04-28 | Carestream Health, Inc. | Method of preparing silver carboxylate soaps |
| US7622247B2 (en) | 2008-01-14 | 2009-11-24 | Carestream Health, Inc. | Protective overcoats for thermally developable materials |
| CN101256346B (zh) * | 2008-02-04 | 2010-09-29 | 黄山银江科技有限公司 | 一种激光照排胶片的生产方法 |
| WO2015148028A1 (en) | 2014-03-24 | 2015-10-01 | Carestream Health, Inc. | Thermally developable imaging materials |
| US9335623B2 (en) | 2014-03-24 | 2016-05-10 | Carestream Health, Inc. | Thermally developable imaging materials |
| WO2016073086A1 (en) | 2014-11-04 | 2016-05-12 | Carestream Health, Inc. | Image forming materials, preparations, and compositions |
| US9523915B2 (en) | 2014-11-04 | 2016-12-20 | Carestream Health, Inc. | Image forming materials, preparations, and compositions |
| WO2016195950A1 (en) | 2015-06-02 | 2016-12-08 | Carestream Health, Inc. | Thermally developable imaging materials and methods |
| US9746770B2 (en) | 2015-06-02 | 2017-08-29 | Carestream Health, Inc. | Thermally developable imaging materials and methods |
| WO2017123444A1 (en) | 2016-01-15 | 2017-07-20 | Carestream Health, Inc. | Method of preparing silver carboxylate soaps |
Also Published As
| Publication number | Publication date |
|---|---|
| GB655082A (en) | 1951-07-11 |
| BE484329A (en)) | |
| FR980385A (fr) | 1951-05-11 |
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