CN1054323A - Direct synthesis technique system concentrated colour bleach-fixing liquid - Google Patents
Direct synthesis technique system concentrated colour bleach-fixing liquid Download PDFInfo
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- CN1054323A CN1054323A CN 90105032 CN90105032A CN1054323A CN 1054323 A CN1054323 A CN 1054323A CN 90105032 CN90105032 CN 90105032 CN 90105032 A CN90105032 A CN 90105032A CN 1054323 A CN1054323 A CN 1054323A
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- fixing liquid
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Abstract
A kind of directly synthetic method for preparing concentrated colour bleach-fixing liquid, it utilizes chloroacetic acid, NaOH, ethylenediamine, ferric trichloride and stop bath ATS (Ammonium thiosulphate) to be raw material, directly makes the required bleach-fixing liquid of colored developing and printing industry.Owing to controlled appropriate reaction conditions, made the reaction conversion ratio height, the stable performance of gained bleach-fixing liquid.With the method ratio of the preparation bleach-fixing liquid of present employing, method for making gained bleach-fixing liquid performance of the present invention reaches the level of the universal product, and the cost of bleach-fixing liquid can significantly drop to and only is the 1/3-1/5 of present used method for making.
Description
The present invention is a kind of preparation method of chemical liquids, exactly be as the synthetic bleached chemical liquid that contains silver-colored oxygenant Ferric Sodium Edetate (calling the EDTA ferrisodium in the following text) and bleaching assistant of base stock by chloroacetic acid, NaOH, ethylenediamine, ferric trichloride etc., mix with stop bath then, make the required bleach-fixing liquid of developing and printing chromophotograph.
The high temperature fast colourful photograph developing and printing technology that grows up the seventies has replaced the oxygenant of the potassium ferricyanide of traditional use as argent with the EDTA ferrisodium after colour development, thereby makes bleaching, photographic fixing two steps operation unite two into one and carry out simultaneously.Promptly be mixed with bleach-fixing liquid, once finish the bleaching and the photographic fixing of chromophotograph by EDTA ferrisodium and ATS (Ammonium thiosulphate).The compound method of practical bleaching liquid is to adopt commodity EDTA ferrisodium and sulfuration ammonium sulfate and other auxiliary agents formulated by a certain percentage mostly.Also can mix by a certain percentage again and be mixed with bleach-fixing liquid with ATS (Ammonium thiosulphate) and other auxiliary agents with EDTA, alkali, ferric trichloride.But, no matter adopt which kind of way preparation bleach-fixing liquid, owing to being base stock, so cost is all very high with EDTA or BDTA ferrisodium.
The purpose of this invention is to provide and a kind ofly directly syntheticly float the method for deciding concentrate, adopt this technology system to float and decide concentrate, need not heat, react on moment to finish.Properties of product are identical with the common bleach-fixing liquid that adopts.And production run is simplified, and shorten reaction time, and raw materials consumption reduces, and the required equipment volume of identical output is dwindled.Thereby cost of products is descended significantly.
The present invention is synthetic to float the method for deciding concentrate and comprises:
1, EDTA ferrisodium bleaching liquid is synthetic;
2, float the preparation of deciding working fluid.
Synthesizing of EDTA ferrisodium bleaching liquid, its chemical reaction is the row reaction equation as follows, the chemical reaction and the indistinction that adopt with common manufacturing process on reactions steps.
Though but be noted that chemical reaction is identical.Because the degree of depth difference that reaction is carried out is so relatively have remarkable difference with current technology.Technology and the not only tediously long complexity of its process of condition according to present industry employing, and as only simplifying the operation course, intermediate product is not made solid and is directly made EDTA ferrisodium solution, then because conversion ratio is low, reaction not exclusively, a large amount of raw materials of not participating in reaction are arranged in the solution, and perhaps intermediate product decomposes in the reaction, thereby can not be directly used in the preparation bleach-fixing liquid.
Direct synthesis process of the present invention, its characteristics are, select and controlled suitable condition in each step reaction.Reaction (1), (2), (3) all can make raw material fully change into required product at short notice, basic free of losses.Thereby can directly synthesize the EDTA ferrisodium bleaching liquid that is used to prepare bleach-fixing liquid.
The present invention synthesizes the desired reaction conditions of EDTA ferrisodium bleaching liquid (float and decide A liquid):
1, the temperature of reaction of reaction (1) is 0～16 ℃;
2, ClCH in the reaction (1)
2COOH: NaOH=1: 1～1.5(mol ratio);
3, ClCH in the reaction (2)
2COONA: H
2NCH
2CH
2NH
2=4: 1～1.2(mol ratio);
4, the temperature of reaction (2) is 50～90 ℃;
5, the pH value of reaction (3) is 8～11.
Its operating process is:
1, certain amount of industrial level chloroacetic acid and water are made solution and be cooled to 0 ℃, add alkali, keep 0～16 ℃ of temperature of reaction;
2, conditioned reaction liquid PH is 8～10, adds a certain amount of technical grade ethylenediamine, makes temperature at 50～90 ℃ under stirring, and falls room temperature naturally then.
3, control PH under 8～11 the condition, in the gained reactant liquor, adds a certain amount of FeCl
3Solution obtains product.
With a certain amount of rapid fixing solution [(NH
4)
2S
2O
3With Na
2S
2O
3Mixed liquor] or ammonia hypo ((NH
4)
2S
2O
3) be added to and make of the present invention floating in the solution of above-mentioned preparation and decide concentrate, be diluted with water to certain concentration solution during use and be common quick bleach-fixing liquid.Below by example technology of the present invention is described further.
The preparation of example 1 EDTA ferrisodium bleaching liquid
Chloroacetic acid 50 gram is dissolved in 100 ml waters, and the control temperature is no more than when adding alkali lye that 40 gram NaOH and 60 ml waters make to PH=9 under 10 ℃ the condition and adds 10 milliliters of ethylenediamines, react 5～10 minutes, and adding remains alkali, then temperature rise to 60 ℃.Reduce to room temperature, stirring down, adding contains FeC
3 6H
231 milliliters of the solution of O1.1g/ce.In adition process, should control reacting system PH value all the time and equal 8.Get 200 milliliters of products at last.EDTAFeNa46g wherein, productive rate 98.5%.
Example two floats decides the working fluid preparation
With 110 gram (NH
4)
2S
2O
3Add and to be mixed into the present invention in 200 ml solns that example one makes and to float and decide concentrate, be diluted to a liter and be to float and decide working fluid.In addition also can get the A of varying number and B as required and mix, dilute and be adjusted to required pH value.
The use experiment of example three synthetic bleach-fixing liquids
Use normal negative, with same printing paper, identical exposure, behind the standard conditions colour display screen, it is fixed to use " Kodak " EP-2 and Japan's " Fuji " bleach-fixing liquid and bleach-fixing liquid of the present invention to float under the same conditions respectively, carries out sensitometry then.
The used strip of sensitometry is with the exposure intensity of red, green, blue three kinds of coloured light to fix, and exposes on a colour paper, makes it after the standard conditions flushing, forms black, white, yellow, green, blue or green multicolored vitta of certain density.Cut in half (finishing identical with assurance) behind this strip colour display screen darkling then, it is fixed to float with contrast bleach-fixing liquid and bleach-fixing liquid of the present invention respectively.Washing, oven dry back are measured strip by red, green, blue three-colour filter respectively with the two light photoelectricity leucometers of Z13-65:
1, white piece reflection density.I.e. Huang, product, blue or green three look photographic fogs.
2, measure blue or green density BR in the black block by red color filter.
3, measure cyan piece density CR by red color filter.
BR-CR=is latent blue or green
Measurement result
| Sample | White piece | Black patch BR | Blue or green piece CR | ||
| R | GT | B | |||
| Bleach-fixing liquid Japanese fuji bleach-fixing liquid of the present invention | 94.7 94.7 | 89.9 90.5 | 87.7 87.7 | 17.5 17.5 | 30.2 30.2 |
| Bleach-fixing liquid of the present invention U.S. Kodak bleach-fixing liquid | 94.8 94.8 | 90.3 90.3 | 88.7 88.7 | 17.5 17.5 | 30.5 30.5 |
The stability experiment of example four bleach-fixing liquids of the present invention
1, EDTAFeNa bleaching liquid
Sample places 20～25 ℃ of placements in the white plastic bottle
| Time | 1 hour | One day | Two days | Three days | 5 days | 30 days | 70 days |
| EDTA% | 15.26 | 15.26 | 15.26 | 15.26 | 15.32 | 16.26 | 15.26 |
2, bleach-fixing liquid of the present invention is stored in the white plastic bottle, and after placing eight months under the room temperature, through the flushing of the same terms, the photograph that washes out is identical with the photograph that " Kodak " bleach-fixing liquid washes out.
Sensitometry result is:
| Sample | White piece | Black patch | Blue or green piece | ||
| Bleach-fixing liquid of the present invention | R 92.5 | G 89.4 | B 87.0 | BR 17.5 | CR 30.2 |
| Kodak's bleach-fixing liquid | 92.5 | 89.4 | 87.0 | 17.5 | 30.2 |
The method for preparing concentrated colour bleach-fixing liquid by the visible direct synthesis technique of the present invention of above-mentioned example, owing to controlled appropriate reaction conditions, utilize chloroacetic acid, NaOH, ethylenediamine, ferric oxide, sulfuration ammonium sulfate to be raw material, directly make required the floating of colored developing and printing industry and decide concentrate.The reaction conversion ratio height, the bleach-fixing liquid stable performance.With the method ratio of present employing, the bleach-fixing liquid performance of the present invention's preparation reaches the level of the universal product, can significantly drop to only for adopting preparation method's 1/3～1/5 at present and float fixed cost.
Claims (4)
1, a kind ofly adds the method that ATS (Ammonium thiosulphate) prepares concentrated colour bleach-fixing liquid, the invention is characterized in: behind the directly synthetic EDTA ferrisodium bleaching liquid of chloroacetic acid, NaOH, ethylenediamine, ferric trichloride, ATS (Ammonium thiosulphate) added make rapid fixing solution.
2, according to the described preparation method who decides concentrate that floats of claim 1, control temperature of reaction at 0～16 ℃ when it is characterized in that the reaction of chloroacetic acid and NaOH, the mol ratio of reactant, chloroacetic acid: NaOH is 1: 1～1.5.
3, according to the described preparation method who decides concentrate that floats of claim 1, the mol ratio that it is characterized in that reactant chloroacetic acid～ethylenediamine is 4: 1～1.2.
4, according to the described preparation method who decides concentrate that floats of claim 1, will control the reactant liquor pH value when it is characterized in that adding ferric oxide is 8～11.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 90105032 CN1029161C (en) | 1990-02-20 | 1990-02-20 | Direct synthesis process of concentrated colour bleaching solution |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 90105032 CN1029161C (en) | 1990-02-20 | 1990-02-20 | Direct synthesis process of concentrated colour bleaching solution |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1054323A true CN1054323A (en) | 1991-09-04 |
| CN1029161C CN1029161C (en) | 1995-06-28 |
Family
ID=4878871
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 90105032 Expired - Fee Related CN1029161C (en) | 1990-02-20 | 1990-02-20 | Direct synthesis process of concentrated colour bleaching solution |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1029161C (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110161798A (en) * | 2017-12-25 | 2019-08-23 | 上海诗淇信息技术有限公司 | A kind of colour bleach-fixing liquid of recyclable regenerative |
-
1990
- 1990-02-20 CN CN 90105032 patent/CN1029161C/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110161798A (en) * | 2017-12-25 | 2019-08-23 | 上海诗淇信息技术有限公司 | A kind of colour bleach-fixing liquid of recyclable regenerative |
| CN110161798B (en) * | 2017-12-25 | 2022-11-15 | 上海诗淇信息技术有限公司 | Recyclable color bleaching and fixing liquid |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1029161C (en) | 1995-06-28 |
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