JPH02262639A - Method for cleaning apparatus for producing silver halide emulsion - Google Patents
Method for cleaning apparatus for producing silver halide emulsionInfo
- Publication number
- JPH02262639A JPH02262639A JP8504189A JP8504189A JPH02262639A JP H02262639 A JPH02262639 A JP H02262639A JP 8504189 A JP8504189 A JP 8504189A JP 8504189 A JP8504189 A JP 8504189A JP H02262639 A JPH02262639 A JP H02262639A
- Authority
- JP
- Japan
- Prior art keywords
- cleaning
- ammonia
- silver nitrate
- pure water
- acid
- 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.)
- Pending
Links
- 238000000034 method Methods 0.000 title claims abstract description 30
- 239000000839 emulsion Substances 0.000 title claims abstract description 23
- 238000004140 cleaning Methods 0.000 title claims abstract description 20
- -1 silver halide Chemical class 0.000 title claims abstract description 18
- 229910052709 silver Inorganic materials 0.000 title claims abstract description 14
- 239000004332 silver Substances 0.000 title claims abstract description 14
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 44
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000004519 manufacturing process Methods 0.000 claims abstract description 9
- 239000002253 acid Substances 0.000 claims abstract description 8
- HAAYBYDROVFKPU-UHFFFAOYSA-N silver;azane;nitrate Chemical compound N.N.[Ag+].[O-][N+]([O-])=O HAAYBYDROVFKPU-UHFFFAOYSA-N 0.000 claims description 9
- 239000002245 particle Substances 0.000 abstract description 25
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 abstract description 20
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 abstract description 15
- 229910017604 nitric acid Inorganic materials 0.000 abstract description 15
- 229910001961 silver nitrate Inorganic materials 0.000 abstract description 10
- 238000007789 sealing Methods 0.000 abstract description 9
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 abstract description 8
- NDVLTYZPCACLMA-UHFFFAOYSA-N silver oxide Chemical compound [O-2].[Ag+].[Ag+] NDVLTYZPCACLMA-UHFFFAOYSA-N 0.000 abstract description 8
- 239000007788 liquid Substances 0.000 abstract description 6
- 229910052736 halogen Inorganic materials 0.000 abstract description 5
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 abstract description 4
- 229910001923 silver oxide Inorganic materials 0.000 abstract description 4
- 229910000147 aluminium phosphate Inorganic materials 0.000 abstract description 2
- 150000002367 halogens Chemical class 0.000 abstract description 2
- XNRABACJWNCNEQ-UHFFFAOYSA-N silver;azane;nitrate Chemical compound N.[Ag+].[O-][N+]([O-])=O XNRABACJWNCNEQ-UHFFFAOYSA-N 0.000 abstract 2
- 150000007513 acids Chemical class 0.000 abstract 1
- 238000007599 discharging Methods 0.000 abstract 1
- 238000004945 emulsification Methods 0.000 abstract 1
- 230000000284 resting effect Effects 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 21
- 239000007864 aqueous solution Substances 0.000 description 17
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 6
- IOLCXVTUBQKXJR-UHFFFAOYSA-M potassium bromide Chemical compound [K+].[Br-] IOLCXVTUBQKXJR-UHFFFAOYSA-M 0.000 description 6
- 108010010803 Gelatin Proteins 0.000 description 5
- 229920000159 gelatin Polymers 0.000 description 5
- 239000008273 gelatin Substances 0.000 description 5
- 235000019322 gelatine Nutrition 0.000 description 5
- 235000011852 gelatine desserts Nutrition 0.000 description 5
- 230000007935 neutral effect Effects 0.000 description 5
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 4
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical compound [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- 235000011114 ammonium hydroxide Nutrition 0.000 description 3
- IYBUGHSUXJVLBQ-UHFFFAOYSA-L dipotassium;bromide;iodide Chemical compound [K+].[K+].[Br-].[I-] IYBUGHSUXJVLBQ-UHFFFAOYSA-L 0.000 description 3
- JKFYKCYQEWQPTM-UHFFFAOYSA-N 2-azaniumyl-2-(4-fluorophenyl)acetate Chemical compound OC(=O)C(N)C1=CC=C(F)C=C1 JKFYKCYQEWQPTM-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 229910021612 Silver iodide Inorganic materials 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 229940045105 silver iodide Drugs 0.000 description 2
- 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 description 2
- 230000002378 acidificating effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 230000005070 ripening Effects 0.000 description 1
- ZUNKMNLKJXRCDM-UHFFFAOYSA-N silver bromoiodide Chemical compound [Ag].IBr ZUNKMNLKJXRCDM-UHFFFAOYSA-N 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明はハロゲン化銀乳剤製造装置の洗浄方法に関する
ものである。DETAILED DESCRIPTION OF THE INVENTION [Field of Industrial Application] The present invention relates to a method for cleaning a silver halide emulsion manufacturing apparatus.
ハロゲン化銀写真感光材料に用いるハロゲン化銀乳剤の
製造には、中性法乳剤（煮沸乳剤、酸性乳剤などと呼ば
れるものを含めて、非アンモニア乳剤）と、アンモニア
法乳剤とに大別される。The production of silver halide emulsions used in silver halide photographic light-sensitive materials is roughly divided into neutral method emulsions (non-ammonia emulsions, including those called boiling emulsions, acidic emulsions, etc.) and ammonia method emulsions. .
中性乳剤は、中性に近い水溶液中で、ハロゲン塩と銀塩
（硝酸銀）を反応させてハロゲン化銀結晶を生成させ、
物理熟成させる方法で、アンモニ、方法乳剤は、ハロゲ
ン塩と銀塩を反応させるとき、アンモニアを共存させる
方法である。アンモニアは、硝酸銀溶液にアンモニア水
を加えて、１度生成する沈澱をさらにアンモニア水を加
えてちょうど溶解させた液（全量アンモニア性硝酸銀溶
液、硝９酸銀１モルに対してアンモニア２モルとなる）
とハロゲン塩を混合させることによって共存させるのが
普通であるが、アンモニアの添加量が全量より少ない場
合（アンモニア性硝酸銀とアンモニアを添加しない硝酸
銀溶液を併用するなど）、ハロゲン塩中にアンモニアを
加える場合などもある。Neutral emulsions are produced by reacting a halide salt and a silver salt (silver nitrate) in a nearly neutral aqueous solution to produce silver halide crystals.
The ammonia emulsion is a physical ripening method in which ammonia is allowed to coexist when a halogen salt and a silver salt are reacted. Ammonia is a solution obtained by adding aqueous ammonia to a silver nitrate solution and dissolving the precipitate that forms once by adding aqueous ammonia (total amount of ammoniacal silver nitrate solution, 2 moles of ammonia per 1 mole of silver nitrate). )
Usually, they are made to coexist by mixing halogen salt with ammonia, but if the amount of ammonia added is less than the total amount (such as when ammoniacal silver nitrate and a silver nitrate solution without ammonia are used together), ammonia is added to the halogen salt. There are also cases.
このようなアンモニア法により、ハロゲン化銀乳剤（以
下、単に乳剤という）を製造する際、アンモニア性硝酸
銀溶液の添加に用いた添加ラインの洗浄にあたり、従来
純水あるいは温純水等により数回にわたり丁寧な洗浄を
行っていた。しかしながら添加ラインの壁に付着したア
ンモニア性硝酸銀溶液は酸化銀を生成し、純水による洗
浄では落ちないことがある。このため品種が切り替わり
た場合に、例えば種乳剤の製造などで、その前にアンモ
ニア法で乳剤仕込みをしｔ；かあるいは中性法で仕込み
をしたかにより不純物（酸化銀）の存在により核の発生
数が異なり結果として、前にアンモニア法を用いなかっ
た場合に比較して、アンモニア法の後では粒径などの変
動を引き起こすことがあった。When silver halide emulsions (hereinafter simply referred to as emulsions) are produced by such an ammonia method, the addition line used for adding the ammoniacal silver nitrate solution has traditionally been carefully washed several times with pure water or hot pure water. I was cleaning. However, ammoniacal silver nitrate solution that adheres to the walls of the addition line produces silver oxide, which may not be removed by washing with pure water. For this reason, when the variety is changed, for example in the production of seed emulsion, the presence of impurities (silver oxide) may cause the nucleus to deteriorate, depending on whether the emulsion was prepared using the ammonia method or the neutral method. The difference in the number of occurrences resulted in variations in particle size etc. after the ammonia method compared to when no ammonia method was used before.
上記のごとき問題に対し、本発明の目的は、アンモニア
法によるハロゲン化銀の製造において、ハロゲン化銀乳
剤粒子を安定に製造できる簡単なアンモニア性硝酸銀溶
液添加ラインの洗浄方法を提供することである。In order to solve the above problems, an object of the present invention is to provide a simple method for cleaning an ammoniacal silver nitrate solution addition line that can stably produce silver halide emulsion grains in silver halide production by the ammonia method. .
本発明の上記目的は、アンモニア法によるハロゲン化銀
乳剤の製造装置において、アンモニア性硝酸銀溶液の添
加ラインを洗浄する場合、酸を使用することを特徴とす
るハロゲン化銀乳剤製造装置の洗浄方法により達成され
る。The above-mentioned object of the present invention is to provide a method for cleaning a silver halide emulsion manufacturing apparatus using an ammonia method, which uses an acid when cleaning an addition line for an ammoniacal silver nitrate solution. achieved.
以下、本発明の詳細について説明する。The details of the present invention will be explained below.
本発明に用いられる酸としては、ハロゲンを含まないも
のが好ましく、硫酸、リン酸、硝酸が挙げられるが硝酸
が最も好ましい・酸の濃度は・希釈せずに用いてもよい
が、安全性、及び後の純水による洗浄の面から１〜３０
％、洗浄能力の面から４０％以上が好ましく、両者を勘
案すれば、２５〜４５％が最も好ましい。The acid used in the present invention is preferably one that does not contain halogen, and examples include sulfuric acid, phosphoric acid, and nitric acid, but nitric acid is the most preferred.The concentration of the acid is.It may be used without dilution, but safety and 1 to 30 in terms of subsequent cleaning with pure water.
%, preferably 40% or more from the viewpoint of cleaning ability, and most preferably 25 to 45%, taking both factors into consideration.
洗浄方法としては、アンモニア法で仕込みを行った後、
硝酸銀溶液の添加ラインに硝酸溶液あるいは硫酸溶液を
入れて、液封放置した後に、これを排出し、最後に純水
で洗浄する。この場合液封時間は４０分以上、好ましく
は６０分以上である。この操作により、純水のみでは取
り除けない酸化銀を取り除くことができ、この後の乳剤
製造を安定に行うことが出来る。As for the cleaning method, after preparing using the ammonia method,
A nitric acid solution or a sulfuric acid solution is put into the addition line of the silver nitrate solution, and after being left in a liquid seal, it is discharged and finally washed with pure water. In this case, the liquid sealing time is 40 minutes or more, preferably 60 minutes or more. By this operation, silver oxide which cannot be removed with pure water alone can be removed, and subsequent emulsion production can be carried out stably.
以下、実施例により本発明の効果を具体的に例証する。 Hereinafter, the effects of the present invention will be specifically illustrated by examples.
実施例１
種粒子の生成
温度を４０℃とした２％のゼラチン水溶液５００ｃｃに
特開昭５０−４５４３７号記載の方法にしたがって、４
．ＯＮ硝酸銀水溶液２５０ｃｃ及び４．ＯＮ臭化カリウ
ム、沃化カリウム（ＫＢｒ：ＫＩ＝９８：２）の混合水
溶液２５０ｃｃをコンドロールドダブルジェット法によ
り、 Ｉ）Ａｇを９．０、ｐＨを２．０に制御しながら
３５分間で添加した。Example 1 500 cc of a 2% aqueous gelatin solution with a seed particle generation temperature of 40°C was mixed with 4
．． 250 cc of ON silver nitrate aqueous solution and 4. I) 250 cc of a mixed aqueous solution of ON potassium bromide and potassium iodide (KBr:KI=98:2) was heated in 35 minutes while controlling Ag to 9.0 and pH to 2.0 using the Chondrold double jet method. Added.
この乳剤をＥｍ−１とする。粒径は０．０９３μｍであ
った。この後、装置の洗浄を純水で行い、次にアンモニ
ア法による粒子の成長を行った。This emulsion is designated as Em-1. The particle size was 0.093 μm. After this, the apparatus was washed with pure water, and then particles were grown by the ammonia method.
粒子成長
以下に示す７種類の溶液を用いて、粒子内部から順次１
５モル％、５モル％、３モル％の沃化銀含有のコア／シ
ェル型で、平均粒径０．３ｇｐ ｍ 、平均沃化銀含有
率８．４６％の沃臭化銀乳剤を作成した。Particle Growth Using the 7 types of solutions shown below, 1.
Core/shell type silver iodobromide emulsions containing 5 mol%, 5 mol%, and 3 mol% of silver iodide, with an average grain size of 0.3 gp m, and an average silver iodide content of 8.46% were prepared. .
以下に示す７種類の溶液を用いた。Seven types of solutions shown below were used.
（Ａ−１）
オセインゼラチン ２８．６ｇグａノ
ン（１０％エタノール水溶液） １６．５騰ａＴ
Ａ Ｉ
２４７．５膳り５６％酢酸水溶液
７２．５１１９２８％アンモニ
ア水溶液
種乳剤
純水で６６０ＦＪａｎにする。(A-1) Ossein gelatin 28.6 g guanone (10% ethanol aqueous solution) 16.5 aT
AI
247.5 servings 56% acetic acid aqueous solution 72.511928% ammonia aqueous solution Seed emulsion Make 660FJan with pure water.
（Ｂ−１） オセインゼラチン 臭化カリウム 沃化カリウム ＡＩ 純水で１３００飄Ｑとする。(B-1) ossein gelatin potassium bromide potassium iodide AI Make it 1300 liters Q with pure water.
（ｃ−１） オセインゼラチン 臭化カリウム 沃化カリウム ＡＩ 純水で１７００−〇とする。(c-1) ossein gelatin potassium bromide potassium iodide AI Adjust to 1700-0 with pure water.
ＣＤ −１）
オセインゼラチン
臭化カリウム
沃化カリウム
Ａｆ
ｇｘ
９７．２鴨Ｑ
０．１５５２モル相当量
１３．０９
４６０．２９
１１３．３９
６７２．６９
４９．３９ｇ
７０１１ｇ
ｇ
３２３．２９
１３．９９
４０擢ｉ
（Ｅ−１）
硝酸銀 １７７３．６９２
８％アンモニア水 １４７０ｍｅ純水
で２９８３ａ＋４とする。CD-1) Ossein gelatin Potassium bromide Potassium iodide Af gx 97.2 Duck Q 0.1552 mole equivalent 13.09 460.29 113.39 672.69 49.39g 7011g g 323.29 13.99 40擢i (E-1) Silver nitrate 1773.692
8% ammonia water Make 2983a+4 with 1470me pure water.
（Ｆ−１）
２０％臭化カリウム水溶液 ｐｈｇ調整必要量（Ｇ
−１）
５６％酢酸水溶液 ｐｔｔ調整必要量（
ＴＡＩ：４−ヒドロキシ−６−メチル−１，３，３ａ、
７−チトラザインデン）４０℃において、撹拌混合機を
用いて溶液Ａ−１に溶液Ｅ−１と溶液Ｂ−１を同時混合
法によって添加した。Ｂ−１添加終了と同時にＣ−１を
添加し、Ｃ−１の添加終了と同時にＤ−１を添加した。(F-1) 20% potassium bromide aqueous solution phg adjustment required amount (G
-1) 56% acetic acid aqueous solution PTT adjustment required amount (
TAI: 4-hydroxy-6-methyl-1,3,3a,
7-chitrazaindene) At 40° C., solution E-1 and solution B-1 were added to solution A-1 by a simultaneous mixing method using a stirring mixer. C-1 was added at the same time as the addition of B-1 was completed, and D-1 was added at the same time as the addition of C-1 was completed.
同時混合中のｐＡｇ％ｐｉ−１の制御および溶液Ｅ−１
、Ｂ−１゜Ｃ−１，Ｄ−１の添加速度は表１のようにし
て行っｌこ 。Control of pAg% pi-1 during simultaneous mixing and solution E-1
, B-1°, C-1, and D-1 were added at the rates shown in Table 1.
表１ この後常法により、脱塩した。Table 1 Thereafter, it was desalted by a conventional method.
以上まで行った後に、アンモニア性硝酸銀溶液の添加ラ
インを
Ａ、純水のみで洗浄した場合。After performing the above steps, the addition line for the ammoniacal silver nitrate solution was cleaned with A, pure water only.
Ｂ、３０％硝酸水溶液を室温で４０分間液封した後、こ
れを排出し、その後純水で洗浄する。B. After sealing with a 30% nitric acid aqueous solution at room temperature for 40 minutes, it is discharged, and then washed with pure water.
の２種類の方法で洗浄し、再び前記種粒子の形成を行っ
た。Ａ、Ｂそれぞれの洗浄後に形成した種粒子をＥ ｍ
−２、Ｅｍ−３とする。これら１連の実験を５回づつ
行った後、Ｅ ｍ −１％Ｅ ｍ −２、Ｅｍ−３の粒
径を比較した。槽内の不純物の種類や量によりハロゲン
化銀の核発生数は大きく変化し、その結果、粒径が変動
すると考えられるため洗浄性を調べるには有効な方法で
ある。The seed particles were washed using two different methods, and the seed particles were formed again. The seed particles formed after washing A and B are E m
-2, Em-3. After conducting each of these series of experiments five times, the particle sizes of Em-1%Em-2 and Em-3 were compared. The number of silver halide nuclei generated varies greatly depending on the type and amount of impurities in the tank, and as a result, the particle size is thought to vary, so this is an effective method for investigating cleaning performance.
この結果を第１図のグラフに示した。The results are shown in the graph of FIG.
第１図は上記５回の実験における粒径の変動を示すグラ
フである。縦軸は粒径（μｍ）、横軸は回数を示す。FIG. 1 is a graph showing the variation in particle size in the five experiments described above. The vertical axis shows the particle size (μm), and the horizontal axis shows the number of times.
第１図の結果から純水のみで洗浄したＥｍ−２に比較し
、洗浄に硝酸溶液を使用したＥ ｍ −３及び中性法に
よるＥｍ−１の場合は粒径変動が著しく少ないことが明
らかである。From the results shown in Figure 1, it is clear that compared to Em-2, which was washed with pure water only, particle size fluctuations were significantly smaller for Em-3, which used a nitric acid solution for washing, and Em-1, which was washed using the neutral method. It is.
実施例２
実施例１において、３０％硝酸水溶液の液封時間を２０
．４０．６０．８０．２１０分と変え、その後に粒子を
形成させた場合のＥｍ−１の粒径（０，０９３μｍ）か
らの変動を調べた。その結果を第２図に示す。Example 2 In Example 1, the sealing time of the 30% nitric acid aqueous solution was 20
．． The variation from the particle size of Em-1 (0,093 μm) was investigated when particles were formed after 40, 60, 80, and 210 minutes. The results are shown in FIG.
！１２図は硝酸水溶液液封時間と粒径変動の関係を示す
グラフである。横軸は液封時間、縦軸は粒径変動を示す
。第２図の結果から液封時間は、３０％硝酸銀溶液の場
合、６０分間以上が好ましいことが分かる。! FIG. 12 is a graph showing the relationship between the sealing time of the nitric acid aqueous solution and the particle size fluctuation. The horizontal axis shows liquid sealing time, and the vertical axis shows particle size fluctuation. From the results shown in FIG. 2, it can be seen that the liquid sealing time is preferably 60 minutes or more in the case of a 30% silver nitrate solution.
実施例３
硝酸水溶液の濃度を変えて６０分間液封した後、純水に
て洗浄を行った後、種粒子を形成した場合のＥｍ−１の
粒径（０，０９３μｍ）からの変動を調べた。その結果
を第３図に示す。第３図は液封した硝酸水溶液の濃度と
粒径変動の関係を示すグラフである。横軸は硝酸水溶液
の濃度を示し、縦軸は粒径変動を示す。ｔｊＪ３図の結
果から硝酸水溶液濃度は３０％以上が好ましいことが分
かる。Example 3 After changing the concentration of the nitric acid aqueous solution and sealing for 60 minutes, washing with pure water, and forming seed particles, the variation from the particle size of Em-1 (0,093 μm) was investigated. Ta. The results are shown in FIG. FIG. 3 is a graph showing the relationship between the concentration of a sealed nitric acid aqueous solution and particle size fluctuation. The horizontal axis shows the concentration of the nitric acid aqueous solution, and the vertical axis shows the particle size variation. From the results shown in Figure tjJ3, it can be seen that the concentration of the nitric acid aqueous solution is preferably 30% or more.
本発明により、アンモニア法によるハロゲン化銀の製造
において、ハロゲン化銀乳剤粒子を安定に製造できる簡
単なアンモニア性硝酸銀添加ラインの洗浄方法を提供す
ることができた。According to the present invention, it has been possible to provide a simple method for cleaning an ammoniacal silver nitrate addition line that can stably produce silver halide emulsion grains in the production of silver halide by the ammonia method.
第１図は洗浄方法の差による粒径変動を示すグラフであ
る。第２図は硝酸水溶液の液封時間による粒径変動に対
する影響を示すグラフである。第３図は液封した硝酸水
溶液濃度の粒径変動に及ぼす影響を示すグラフである。FIG. 1 is a graph showing particle size variations due to differences in cleaning methods. FIG. 2 is a graph showing the influence of the sealing time of a nitric acid aqueous solution on particle size fluctuations. FIG. 3 is a graph showing the influence of the concentration of a sealed nitric acid aqueous solution on particle size fluctuations.
Claims (1)
て、アンモニア性硝酸銀溶液の添加ラインを洗浄する場
合、純水洗浄前に酸を使用することを特徴とするハロゲ
ン化銀乳剤製造装置の洗浄方法。1. A method for cleaning a silver halide emulsion manufacturing apparatus using an ammonia method, which comprises using an acid before cleaning with pure water when cleaning an addition line for an ammoniacal silver nitrate solution.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP8504189A JPH02262639A (en) | 1989-04-03 | 1989-04-03 | Method for cleaning apparatus for producing silver halide emulsion |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP8504189A JPH02262639A (en) | 1989-04-03 | 1989-04-03 | Method for cleaning apparatus for producing silver halide emulsion |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH02262639A true JPH02262639A (en) | 1990-10-25 |
Family
ID=13847604
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP8504189A Pending JPH02262639A (en) | 1989-04-03 | 1989-04-03 | Method for cleaning apparatus for producing silver halide emulsion |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH02262639A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0706801A1 (en) | 1994-10-12 | 1996-04-17 | Fuji Photo Film Co., Ltd. | Method for sterilizing apparatus for preparation of recording material |
-
1989
- 1989-04-03 JP JP8504189A patent/JPH02262639A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0706801A1 (en) | 1994-10-12 | 1996-04-17 | Fuji Photo Film Co., Ltd. | Method for sterilizing apparatus for preparation of recording material |
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