CN101256346B - Method for producing laser photo film - Google Patents
Method for producing laser photo film Download PDFInfo
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- CN101256346B CN101256346B CN2008100205985A CN200810020598A CN101256346B CN 101256346 B CN101256346 B CN 101256346B CN 2008100205985 A CN2008100205985 A CN 2008100205985A CN 200810020598 A CN200810020598 A CN 200810020598A CN 101256346 B CN101256346 B CN 101256346B
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- lotion
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- sedimentation
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Abstract
The invention discloses a producing method of laser phototypesetting film, comprising double-pour emulsifying step, edulcorating step, curing step and coating step. The edulcorating step comprises a) sedimentating step, b) washing step, c) remelting step, d) sedimentating step, e) washing step, f) remelting step. A variety of purities in the emulsion are removed using more than once remelting step and the control method is easy without adding device. The property of each emulsion is stable and the coating quality and stability of film is good.
Description
Technical field
The invention belongs to the production method of laser photo film, belong to production method especially with the laser photo film of high chlorine emulsion emulsification.
Background technology
Laser photo film comprises He-Ne Lasers phototypesetting sheet, infrared laser phototypesetting sheet, and the production method of laser photo film comprises two emulsification process of annotating at present, removal of impurities operation, curing step, and painting process:
Described two emulsification process of annotating: in uniform temperature, under the situation of high-speed stirred, constant maintenance halogen ion is excessive, with silver nitrate (AgNO
3) solution and alkali halide solution join in the aqueous gelatin solution with constant speed simultaneously, alkali halide is sodium chloride, potassium bromide or sodium chloride, potassium bromide, potassium iodide, in alkali halide, mix up iridium salt is arranged, rhodium salt.
Described removal of impurities operation: comprise sedimentation operation, washing step, redissolution operation:
Washing step: the conductivity＜800 μ S/cm that are washed to film;
Redissolution operation: use Na
2CO
3Solution dissolving lotion is regulated PH=4.7 ± 0.2 with acetic acid again;
Described painting process: lotion sulphur, gold with curing step made are coated with sample after the red sensitive dye sensitizing.
Usually the coating of laser photo film is thinner, because the prepared emulsion of two notes emulsification process is high chlorine emulsion, in the painting process process, when the impurity element of high chlorine emulsion is too much, can cause the film surface to have defective.The impurity element of common high chlorine emulsion mainly comprises the following aspects: 1, in high chlorine emulsion preparation process, because perchloric acid is to the corrosion of equipment, can stay a large amount of ferric ions in the emulsion, ferric ion directly influences the photographic fog and the light sensitivity of film, and is very unfavorable to the preservation and the production of film; 2, the used emulsion bases of high chlorine emulsion is a gelatin, inorganic salts in the emulsion such as sodium nitrate, and potassium nitrate, alkaline halide are adsorbed by gelatin easily, are difficult for cleaning up; 3, various production starting material itself just contain micro impurity element, as Au, Hg, Fe, Cr, Ni, Mn, Cu and sulfide, when using the raw material in different times, the place of production, cause the difference of impurity element in the high chlorine emulsion easily, make the character of different batches laser photo film produce difference, during with the method for preparing laser photo film, the loss in weight of silver is all more than 3% in the film, and printing cost is higher.
Summary of the invention
Technical matters to be solved by this invention provides the production method of the laser photo film that a kind of impurity element is few, cost is low.
The technical scheme of technical solution problem of the present invention is: a kind of production method of laser photo film, comprise two emulsification process of annotating, and removal of impurities operation, curing step, painting process, described removal of impurities operation comprises following operation:
A) sedimentation operation: the used sinking agent of sedimentation operation is a naphthalene sulfonate, and the weight ratio of sinking agent and gelatin is 1: 5-10.
Naphthalene sulfonate is present general sinking agent, when the weight ratio of sinking agent and gelatin is 1: during 5-20, making high chlorine emulsion can sedimentation be blocks of solid, help cleaning, and the loss of silver is less in the cleaning process, but when the weight ratio of sinking agent and gelatin when being 1: 5, then make high chlorine emulsion the colloidal solid that is difficult to redissolve occur.
B) washing step: regulate PH=3.5 ± 0.2 of lotion, leave standstill, take out supernatant liquor, stir down and use pure water to wash, be washed to the conductivity＜800 μ S/cm of lotion;
The gelatin that adds sinking agent loses water wettability owing to amino with the sulfonic group complexing, thereby reach the effect of sedimentation, when pH value transfers to the isoelectric point of gelatin when following, carboxyl also loses water wettability, gelatin is just together with the silver halide particle sedimentation, most of impurity salt is dissolved in the water and is removed, and the heavy phenomenon of silver occurs if pH value is crossed low meeting, produces irreversible destruction for emulsion systems.
C) redissolution operation: add Na
2CO
3Solution is warmed up to 38-40 ℃, and paste dissolves is got final product;
D) sedimentation operation: at c) add sinking agent in the redissolution solution that operation generated, used sinking agent is a naphthalene sulfonate, and the weight ratio of sinking agent and gelatin is 1: 10-20;
The amount ratio a operation much less of the sinking agent of this operation is to be adsorbed on inorganic salts in the gelatin, and the impurity element of trace in order to remove because the sinking agent that adds in a operation also in emulsion, increases this process.
E) washing step: regulate PH=3.5 ± 0.2 of lotion, leave standstill, take out supernatant liquor, stir down and use pure water to wash, be washed to the conductivity＜800 μ S/cm of lotion;
F) redissolution operation: in the good lotion of washing, add Na
2CO
3Solution is warmed up to 38-40 ℃, adds gelatin, stirring and dissolving.Regulate PH=4.7 ± 0.2 of lotion, get final product;
Also should add an amount of gelatin after the redissolution operation, the amount of adding gelatin has different requirements according to different prescriptions, and for lithographic film emulsion, glue silver is better more than low more, and this is to the attenuate coating, and good action has promoted clearness.But cross low glue silver than can guarantee system stable, the heavy phenomenon of silver appears, unfavorable to producing.
In order to strengthen impurity-eliminating effect, also can carry out once above d, e, f operation.
The emulsion sedimentation is to rely on the hydrophilic radical that changes gelatin, gelatin no longer is dissolved in the water and reaches the purpose of cleaning, at this time can be wrapped in the gelatin that is not dissolved in water by some impurity, because the gelatin of impurity outside exists, be unfavorable for contacting of pure water and impurity, tradition relies on repeatedly to be washed and measures the washing water conductivity after the sedimentation to control the scheme of washing degree just powerless to this part impurity.Emulsion after the washing redissolves the impurity that is wrapped in gelatin inside is dissolved in the solution, can remove impurity preferably after the sedimentation, and inner impurity content is further reduced.
The present invention compared with prior art adopts once above method of redissolving to remove the plurality of impurities of deemulsifying agent the inside, and control method is fairly simple, does not increase equipment, can guarantee every batch of emulsion stable performance, and the stability of coating quality and film better.
Embodiment
Below in conjunction with embodiment the present invention is done detailed explanation.
Embodiment 1:
A kind of production method of laser photo-typesetting emulsion comprises two emulsification process of annotating, removal of impurities operation, curing step, and painting process, described removal of impurities operation comprises following operation:
A) sedimentation operation: the used sinking agent of sedimentation operation is a naphthalene sulfonate, and the weight ratio of sinking agent and gelatin is 1: 10;
B) washing step: regulate PH=3.5 ± 0.2 of lotion with acetic acid, leave standstill 5 minutes after, take out supernatant liquor, stir and use pure water that sedimentation emulsion is washed down, be washed to the conductivity＜800 μ S/cm of lotion;
C) redissolution operation: add Na
2CO
3Solution is warmed up to 38-40 ℃, and paste dissolves is got final product;
D) sedimentation operation: at c) add sinking agent in the redissolution solution that operation generated, used sinking agent is a naphthalene sulfonate, and the weight ratio of sinking agent and gelatin is 1: 20.
E) washing step; Regulate PH=3.5 ± 0.2 of lotion with acetic acid, leave standstill 5 minutes after, take out supernatant liquor, stir and use pure water that sedimentation emulsion is washed down, be washed to the conductivity＜800 μ S/cm of lotion;
F) redissolution operation: in the good lotion of washing, add Na
2CO
3Solution is warmed up to 38-40 ℃, adds gelatin, stirring and dissolving, and acetic acid is regulated PH=4.7 ± 0.2 of lotion, gets final product.
Embodiment 2:
A kind of production method of laser photo-typesetting emulsion comprises two emulsification process of annotating, removal of impurities operation, ripe operation, and painting process, described removal of impurities operation comprises following operation:
A) sedimentation operation: the used sinking agent of sedimentation operation is a naphthalene sulfonate, and the weight ratio of sinking agent and gelatin is 1: 8;
B) washing step: regulate PH=3.5 ± 0.2 of lotion with acetic acid, leave standstill 5 minutes after, take out supernatant liquor, stir and use pure water that sedimentation emulsion is washed down, be washed to the conductivity＜800 μ S/cm of lotion;
C) redissolution operation: add Na
2CO
3Solution is warmed up to 38-40 ℃, and paste dissolves is got final product;
D) sedimentation operation: at c) add sinking agent in the redissolution solution that operation generated, used sinking agent is a naphthalene sulfonate, and the weight ratio of sinking agent and gelatin is 1: 20.
E) washing step; Regulate PH=3.5 ± 0.2 of lotion with acetic acid, leave standstill 5 minutes after, take out supernatant liquor, stir and use pure water that sedimentation emulsion is washed down, be washed to the conductivity＜800 μ S/cm of lotion;
F) redissolution operation: in the good lotion of washing, add Na
2CO
3Solution is warmed up to 38-40 ℃, adds gelatin, stirring and dissolving, and acetic acid is regulated PH=4.7 ± 0.2 of lotion, gets final product.
Embodiment 3:
A kind of production method of laser photo-typesetting emulsion comprises two emulsification process of annotating, removal of impurities operation, ripe operation, and painting process, described removal of impurities operation comprises following operation:
A) sedimentation operation: the used sinking agent of sedimentation operation is a naphthalene sulfonate, and the weight ratio of sinking agent and gelatin is 1: 9;
B) washing step: use acetic acid to regulate PH=3.5 ± 0.2 of lotion, leave standstill 5 minutes after, take out supernatant liquor, stir and use pure water that sedimentation emulsion is washed down, be washed to the conductivity＜800 μ S/cm of lotion;
C) redissolution operation: add Na
2CO
3Solution is warmed up to 38-40 ℃, and paste dissolves is got final product;
D) sedimentation operation: at c) add sinking agent in the redissolution solution that operation generated, used sinking agent is a naphthalene sulfonate, and the weight ratio of sinking agent and gelatin is 1: 20.
E) washing step; Use acetic acid to regulate PH=3.5 ± 0.2 of lotion, leave standstill 5 minutes after, take out supernatant liquor, stir and use pure water to wash down, be washed to the conductivity＜800 μ S/cm of lotion;
F) redissolution operation: in the good lotion of washing, add Na
2CO
3Solution is warmed up to 38-40 ℃, adds gelatin, stirring and dissolving.Use acetic acid to regulate PH=4.7 ± 0.2 of lotion, get final product.
Embodiment 4:
A kind of production method of laser photo-typesetting emulsion comprises two emulsification process of annotating, removal of impurities operation, ripe operation, and painting process, described removal of impurities operation comprises following operation:
A) sedimentation operation: the used sinking agent of sedimentation operation is a naphthalene sulfonate, and the weight ratio of sinking agent and gelatin is 1: 10;
B) washing step: regulate PH=3.5 ± 0.2 of lotion with nitric acid, leave standstill 5 minutes after, take out supernatant liquor, stir and use pure water that sedimentation emulsion is washed down, be washed to the conductivity＜800 μ S/cm of lotion;
C) redissolution operation: add Na
2CO
3Solution is warmed up to 38-40 ℃, and paste dissolves is got final product;
D) sedimentation operation: at c) add sinking agent in the redissolution solution that operation generated, used sinking agent is a naphthalene sulfonate, and the weight ratio of sinking agent and gelatin is 1: 20.
E) washing step; Use nitric acid to regulate PH=3.5 ± 0.2 of lotion, leave standstill 5 minutes after, take out supernatant liquor, stir and use the capable washing of pure water down, be washed to the conductivity＜800 μ S/cm of lotion;
F) redissolution operation: in the good lotion of washing, add Na
2CO
3Solution is warmed up to 38-40 ℃, adds gelatin, and stirring and dissolving uses nitric acid to regulate PH=4.7 ± 0.2 of lotion, gets final product;
G) sedimentation operation: at f) add sinking agent in the redissolution solution that operation generated, used sinking agent is a naphthalene sulfonate, and the weight ratio of sinking agent and gelatin is 1: 30.
H) washing step; Use nitric acid to regulate the PH=4.0 of lotion, leave standstill 5 minutes after, take out supernatant liquor, stir and use the capable washing of pure water down, be washed to the conductivity＜800 μ S/cm of lotion;
I) redissolution operation: in the good lotion of washing, add Na
2CO
3Solution is warmed up to 38-40 ℃, adds gelatin, and stirring and dissolving uses nitric acid to regulate PH=4.7 ± 0.2 of lotion, gets final product.
Embodiment 5:
A kind of production method of laser photo-typesetting emulsion comprises two emulsification process of annotating, removal of impurities operation, ripe operation, painting process, and described removal of impurities operation comprises following operation:
A) sedimentation operation: the used sinking agent of sedimentation operation is a naphthalene sulfonate, and the weight ratio of sinking agent and gelatin is 1: 10;
B) washing step: acetic acid is regulated pH value to PH=3.5 ± 0.2, leaves standstill after 5 minutes and takes out supernatant liquor, uses pure water that sedimentation emulsion is washed, and is washed to the conductivity＜800 μ S/cm of lotion;
F) redissolution operation: in the good lotion of washing, add Na
2CO
3Solution is warmed up to 38-40 ℃, and acetic acid is regulated PH=4.7 ± 0.2 of lotion, gets final product.
To two maturations under the above-mentioned example similarity condition, the red sensitive dye spectral sensitization is added antifoggant, and surfactant etc. are coated with sample.
The performance of the existing sample preparation sheet of embodiment 1-5 is as shown in table 1.
Conditions of exposure: intensity-scale type exposure instrument, light source color temperature: 2856K, thunder step on 25 color filter, 3/20 second time shutter.
Washing condition:
| Program | Time, S | Temperature, ℃ | The processing soup |
| Develop | 60 | 32±0.5 | D-11 |
| Photographic fixing | 60 | 32±0.5 | F-5 |
| Washing | 60 | Room temperature | --- |
| Dry | --- | ＜45 | --- |
Developer solution D-11 is p-dihydroxy-benzene, 30 gram natrium carbonicum calcinatums, 1.0 gram Mitouer, the 5.0 gram potassium bromides that every liter of solution contains 105 gram anhydrous sodium sulfites, 9.0 grams.
The performance that the print that embodiment 1-5 is made is placed after 1 year naturally is as shown in table 2.
D
0, γ, S, D
MaxDetect according to the HG/T2172-1991 standard.
The loss of silver amount detects by test emulsion silver content.
Table 1
| Project | D 0 | γ | S | D max | The loss of silver amount |
| Embodiment 1 | 0.04 | 5.2 | 1.2 | 4.25 | 1.7％ |
| Project | D 0 | γ | S | D max | The loss of silver amount |
| Embodiment 2 | 0.04 | 5.6 | 1.3 | 4.19 | 2.1％ |
[0076]
| Embodiment 3 | 0.04 | 5.5 | 1.0 | 4.06 | 2.6％ |
| Embodiment 4 | 0.04 | 5.5 | 1.2 | 4.13 | 1.1％ |
| Embodiment 5 | 0.04 | 6.0 | 1.0 | 4.62 | 3.6％ |
Table 2 (placing measurement performance after a year naturally)
| Project | D 0 | γ | S | D max |
| Embodiment 1 | 0.06 | 5.0 | 1.6 | 4.62 |
| Embodiment 2 | 0.06 | 5.3 | 1.5 | 4.37 |
| Embodiment 3 | 0.05 | 5.0 | 1.5 | 4.45 |
| Embodiment 4 | 0.06 | 5.1 | 1.3 | 4.28 |
| Embodiment 5 | 0.08 | 5.0 | 1.8 | 4.31 |
As seen from Table 1 and Table 2, the method that secondary redissolves improves the production stability and the storage stability of lithographic film, and can effectively control the silver consumption.
Claims (1)
1. the production method of a laser photo film comprises two emulsification process, removal of impurities operation, curing step, painting process annotated, and it is characterized in that: described removal of impurities operation comprises following operation:
A) sedimentation operation: the used sinking agent of sedimentation operation is a naphthalene sulfonate, and the weight ratio of sinking agent and gelatin is 1: 5-10;
B) washing step: regulate PH=3.5 ± 0.2 of lotion, leave standstill, take out supernatant liquor, stir down and use pure water to wash, be washed to the conductivity＜800 μ S/cm of lotion;
C) redissolution operation: add Na
2CO
3Solution is warmed up to 38-40 ℃, and paste dissolves is got final product;
D) sedimentation operation: at c) add sinking agent in the redissolution solution that operation generated, used sinking agent is a naphthalene sulfonate, and the weight ratio of sinking agent and gelatin is 1: 10-20;
E) washing step: regulate PH=3.5 ± 0.2 of lotion, leave standstill, take out supernatant liquor, stir down and use pure water to wash, be washed to the conductivity＜800 μ S/cm of lotion;
F) redissolution operation: in the good lotion of washing, add Na
2CO
3Solution is warmed up to 38-40 ℃, adds gelatin, stirring and dissolving, and PH=4.7 ± 0.2 of adjusting lotion gets final product.
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|---|---|---|---|
| CN2008100205985A CN101256346B (en) | 2008-02-04 | 2008-02-04 | Method for producing laser photo film |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008100205985A CN101256346B (en) | 2008-02-04 | 2008-02-04 | Method for producing laser photo film |
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|---|---|
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| CN101256346B true CN101256346B (en) | 2010-09-29 |
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2489341A (en) * | 1944-07-04 | 1949-11-29 | Ilford Ltd | Production of photographic silver halide emulsions |
| US2614928A (en) * | 1947-08-13 | 1952-10-21 | Eastman Kodak Co | Method of preparing photographic emulsions |
| US2618556A (en) * | 1947-11-19 | 1952-11-18 | Eastman Kodak Co | Process for preparing photographic emulsions |
| CN1095166A (en) * | 1994-02-23 | 1994-11-16 | 中国科学院感光化学研究所 | A kind of method that improves photosensitivity of silver chloride emulsion |
| EP0645672A1 (en) * | 1993-09-23 | 1995-03-29 | Minnesota Mining And Manufacturing Company | Method for preparing silver halide photographic emulsions |
| US5977190A (en) * | 1998-01-14 | 1999-11-02 | Eastman Kodak Company | Process for deionizing and concentrating emulsions |
| CN1932641A (en) * | 2005-09-16 | 2007-03-21 | 中国科学院理化技术研究所 | Plate shape silver halide emulsion adapted to ray photography, producing method and use thereof |
-
2008
- 2008-02-04 CN CN2008100205985A patent/CN101256346B/en not_active Expired - Fee Related
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2489341A (en) * | 1944-07-04 | 1949-11-29 | Ilford Ltd | Production of photographic silver halide emulsions |
| US2614928A (en) * | 1947-08-13 | 1952-10-21 | Eastman Kodak Co | Method of preparing photographic emulsions |
| US2618556A (en) * | 1947-11-19 | 1952-11-18 | Eastman Kodak Co | Process for preparing photographic emulsions |
| EP0645672A1 (en) * | 1993-09-23 | 1995-03-29 | Minnesota Mining And Manufacturing Company | Method for preparing silver halide photographic emulsions |
| CN1095166A (en) * | 1994-02-23 | 1994-11-16 | 中国科学院感光化学研究所 | A kind of method that improves photosensitivity of silver chloride emulsion |
| US5977190A (en) * | 1998-01-14 | 1999-11-02 | Eastman Kodak Company | Process for deionizing and concentrating emulsions |
| CN1932641A (en) * | 2005-09-16 | 2007-03-21 | 中国科学院理化技术研究所 | Plate shape silver halide emulsion adapted to ray photography, producing method and use thereof |
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|---|---|
| CN101256346A (en) | 2008-09-03 |
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