JPH05107668A - Apparatus for producing silver halide photographic emulsion - Google Patents
Apparatus for producing silver halide photographic emulsionInfo
- Publication number
- JPH05107668A JPH05107668A JP29494191A JP29494191A JPH05107668A JP H05107668 A JPH05107668 A JP H05107668A JP 29494191 A JP29494191 A JP 29494191A JP 29494191 A JP29494191 A JP 29494191A JP H05107668 A JPH05107668 A JP H05107668A
- Authority
- JP
- Japan
- Prior art keywords
- silver halide
- diameter
- stirring blade
- liquid flow
- cylinder
- 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.)
- Granted
Links
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明はハロゲン化銀写真乳剤の
製造装置に関する。さらに詳しくは大量製造の場合にも
粒子径分布がせまく、かつ粒子晶癖の均一なハロゲン化
銀粒子を製造することができるハロゲン化銀写真乳剤製
造装置に関する。FIELD OF THE INVENTION The present invention relates to an apparatus for producing a silver halide photographic emulsion. More specifically, the present invention relates to a silver halide photographic emulsion production apparatus capable of producing silver halide grains having a narrow grain size distribution and a uniform grain habit even in the case of mass production.
【０００２】[0002]
【従来の技術】一般的にハロゲン化銀粒子は、反応容器
中のコロイド水溶液において、銀塩水溶液とハロゲン塩
水溶液とを反応させることにより製造される。反応溶液
中にゼラチンのような保護コロイドおよびハロゲン塩水
溶液を入れ、これに銀塩水溶液をある時間添加するシン
グルジェット法や、反応容器中にゼラチン水溶液を入れ
ハロゲン塩水溶液と銀塩水溶液とをそれぞれある時間添
加するダブルジェット法が知られている。両者を比較す
ると、ダブルジェット法の方が粒子径分布の狭いハロゲ
ン化銀粒子が得られ、さらに粒子の成長に伴って、その
ハライド組成を自由に変えることができる点で有利とさ
れており、このダブルジェット法によるハロゲン化銀写
真乳剤の製造装置として、米国特許第３，４１５，６５
０号明細書、英国特許第１，３２３，４６４号明細書、
米国特許第３，６９２，２８３号明細書、特公昭５５−
１０５４５号公報等に開示された技術が知られている。2. Description of the Related Art Generally, silver halide grains are produced by reacting a silver salt aqueous solution with a halogen salt aqueous solution in a colloidal aqueous solution in a reaction vessel. A single jet method in which a protective colloid such as gelatin and an aqueous solution of a halogen salt are placed in a reaction solution, and the aqueous solution of a silver salt is added thereto for a certain period of time, or an aqueous solution of gelatin is placed in a reaction vessel to separate an aqueous solution of a halogen salt and an aqueous solution of a silver salt, respectively. A double jet method is known in which it is added for a certain period of time. Comparing the two, the double jet method is considered to be advantageous in that a silver halide grain having a narrow grain size distribution can be obtained, and further the halide composition can be freely changed with the growth of the grain, An apparatus for producing a silver halide photographic emulsion by the double jet method is disclosed in US Pat. No. 3,415,65.
No. 0, British Patent No. 1,323,464,
U.S. Pat. No. 3,692,283, Japanese Patent Publication No. 55-
The technique disclosed in Japanese Patent No. 10545 is known.
【０００３】これらの装置は銀塩水溶液とハロゲン塩水
溶液の均一な反応条件を生み出すために、さらにはハロ
ゲン化銀写真乳剤の製造工程の簡易化を図るために考案
されたもので、混合器の形状、ハロゲン塩水溶液および
銀塩水溶液の供給方法等に改良を加えたものである。し
かしながらこれらの技術では反応容器内全体における液
の循環流の均一性に欠ける等の欠点により、充分に粒子
径分布が狭くかつ粒子晶癖の均一なハロゲン化銀粒子を
製造することは困難である。一方、特開昭５７−９２５
２４号公報には反応容器内全体における液の循環流の均
一化を攪拌翼による吐出流を液流規制板によって鉛直流
主体の流れに変換することによって改善するハロゲン化
銀乳剤の製造装置が開示されている。しかしながらこの
技術によっても液の循環性はまだ充分でなく、粒子径分
布の充分に狭いハロゲン化銀粒子を製造することができ
なかった。These devices were designed to produce uniform reaction conditions between the aqueous silver salt solution and the aqueous halogen salt solution, and also to simplify the manufacturing process of the silver halide photographic emulsion. The shape and the method of supplying the aqueous solution of halogen salt and the aqueous solution of silver salt are improved. However, with these techniques, it is difficult to produce silver halide grains having a sufficiently narrow grain size distribution and a uniform grain habit due to drawbacks such as lack of uniformity in the circulating flow of the liquid in the entire reaction vessel. .. On the other hand, JP-A-57-925
Japanese Unexamined Patent Publication (Kokai) No. 24 discloses an apparatus for producing a silver halide emulsion, which improves the homogenization of the circulation flow of the liquid in the entire reaction vessel by converting the discharge flow by the stirring blade into a flow mainly composed of vertical direct current by a liquid flow regulating plate. Has been done. However, even with this technique, the circulation of the liquid is still insufficient, and silver halide grains having a sufficiently narrow grain size distribution cannot be produced.
【０００４】液の循環性を改良し粒子径分布が狭く、か
つ粒子晶癖の均一なハロゲン化銀粒子を製造できる装置
として実公平３−２０８２９号公報に、さらに前記のハ
ロゲン化銀粒子を多量に製造できる装置として特公平２
−６０１６６号公報にて開示されたハロゲン化銀写真乳
剤の製造装置にて一応の目的は達せられたものの、さら
に大量のハロゲン化銀写真乳剤を製造する場合には（た
とえば１０００リットル以上の反応容器で製造する場合
や４０００ｃｃ／分以上の流量でハロゲン塩水溶液およ
び銀塩水溶液を混合容器に供給する場合等）、前記特公
平２−６０１６６号公報に示された装置であっても、混
合容器の大きさや攪拌翼回転速度が適正範囲を大きく逸
脱し機械的に製作困難であるため、充分な循環流が得ら
れず所望するハロゲン化銀粒子を得ることができなかっ
た。As a device capable of producing a silver halide grain having an improved liquid circulation property and a narrow grain size distribution and a uniform grain habit, Japanese Utility Model Publication No. 3-208829 discloses a large amount of the above-mentioned silver halide grains. As a device that can be manufactured in Japan
Although the silver halide photographic emulsion manufacturing apparatus disclosed in JP-A-60166 has achieved its intended purpose, in the case of manufacturing a larger amount of silver halide photographic emulsion (for example, a reaction vessel of 1000 liters or more). In the case of supplying the halogen salt aqueous solution and the silver salt aqueous solution to the mixing container at a flow rate of 4000 cc / min or more), even if the apparatus disclosed in Japanese Patent Publication No. 2-60166 is used. Since the size and the rotating speed of the stirring blade largely deviate from the proper range and mechanical production is difficult, a sufficient circulation flow cannot be obtained and desired silver halide grains cannot be obtained.
【０００５】本発明の目的は、粒子径分布が狭く、かつ
粒子晶癖の均一なハロゲン化銀粒子を大量に製造できる
装置を提供することにある。An object of the present invention is to provide an apparatus capable of producing a large amount of silver halide grains having a narrow grain size distribution and a uniform grain habit.
【０００６】[0006]
【課題を解決するための手段】上記課題は、ダブルジェ
ット法によるハロゲン化銀粒子製造装置において、反応
容器中に、翼の遠心方向ないし斜め下方に液流を生ぜし
める攪拌翼と、その周囲に固定された前記攪拌翼径の
１．１ないし１．５倍の直径を有する円筒と、該円筒の
上端部より離れた位置に配置され攪拌翼回転軸下方向の
液流を規制し液面からの空気混入を抑制する前記円筒と
ほぼ同径の液流規制板と、前記攪拌翼の下方に位置し上
方にハロゲン塩水溶液および銀塩水溶液を吐出する注入
ノズルとから成ることを特徴とするハロゲン化銀写真乳
剤の製造装置で、攪拌翼の直径は反応容器直径の２０％
ないし３０％としたハロゲン化銀写真乳剤製造装置によ
り達成することができた。SUMMARY OF THE INVENTION In a silver halide grain producing apparatus by the double jet method, the above-mentioned problem is solved. In a reaction vessel, a stirring blade for generating a liquid flow in a centrifugal direction or obliquely downward of the blade and a surrounding of the stirring blade are provided. A fixed cylinder having a diameter of 1.1 to 1.5 times the diameter of the stirring blade, and a liquid cylinder that is arranged at a position distant from the upper end of the cylinder and regulates the liquid flow in the downward direction of the rotation axis of the stirring blade from the liquid surface. A liquid flow restricting plate having substantially the same diameter as that of the cylinder for suppressing air entrainment, and an injection nozzle located below the stirring blade and discharging a halogen salt aqueous solution and a silver salt aqueous solution upward. The diameter of the stirring blade is 20% of the diameter of the reaction vessel in the silver halide photographic emulsion manufacturing equipment.
It could be achieved by using a silver halide photographic emulsion manufacturing apparatus having a content of ˜30%.
【０００７】[0007]
【実施例および作用】図１は、本発明の一実施例を示す
模式構成図である。便宜上、攪拌翼周辺については斜視
図とした。１は反応容器であらかじめ保護コロイド水溶
液が満たされており、該水溶液の液面は少なくとも攪拌
翼３より上面、さらに好ましくは液流規制板５よりも上
面になるように満たされている。本発明においては攪拌
翼３はピッチドタービン型やピッチドパドル型のもの
等、回転させることにより翼に対して遠心方向ないしは
斜め下方へ吐出される液流が生じるものを使用するが、
攪拌翼３に対する液供給側に注目すると回転軸に沿って
上方からの攪拌翼３への急激な下方流が観察できる。仮
に、図１に示す液流規制板５が存在しない場合は前記の
急激な下方流は回転軸付近の液面を凹ならしめ、多量の
空気を液中に混入させおびただしい発泡を引き起こす。
発泡はハロゲン化銀写真乳剤製造において、均一なハロ
ゲン化銀粒子の形成ないしは成長に対し著しい妨げとな
るほか、乳剤収率の面からも好ましくないものである。
本発明の如く液流規制板５を配備することにより、回転
軸付近の液面が凹むことを防止し、発泡を抑制すること
が可能となる。この結果、液流規制板５の下面側で放射
方向から回転軸に向かう液流も形成されるに至る。この
ことは、本発明のように銀塩水溶液およびハロゲン塩水
溶液を連続的に注入し攪拌混合して生成されたハロゲン
化銀粒子を攪拌翼の吐出流にのせて反応容器内のコロイ
ド水溶液に分散させたあと、反応容器内の液循環により
再び銀塩水溶液およびハロゲン塩水溶液の攪拌混合に供
されるというリサイクル型のハロゲン化銀粒子の成長過
程において、該リサイクル周期の短縮化および粒子間の
リサイクル周期の差を少なくさせて、均一に粒子成長を
促進させる効果がうまれる。DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS FIG. 1 is a schematic block diagram showing an embodiment of the present invention. For convenience, a perspective view is shown around the stirring blade. Reference numeral 1 denotes a reaction vessel which is previously filled with a protective colloid aqueous solution, and the liquid level of the aqueous solution is filled at least above the stirring blades 3, and more preferably above the liquid flow regulating plate 5. In the present invention, the stirring blade 3 is of a pitched turbine type, a pitched paddle type, or the like, which is rotated to generate a liquid flow discharged in a centrifugal direction or obliquely downward with respect to the blade.
Focusing on the liquid supply side with respect to the stirring blade 3, a rapid downward flow from above to the stirring blade 3 can be observed along the rotation axis. If the liquid flow restricting plate 5 shown in FIG. 1 does not exist, the abrupt downward flow causes the liquid surface near the rotating shaft to be concave, causing a large amount of air to be mixed into the liquid and causing enormous bubbling.
Foaming significantly hinders the formation or growth of uniform silver halide grains in the production of a silver halide photographic emulsion, and is not preferable in terms of emulsion yield.
By disposing the liquid flow restricting plate 5 as in the present invention, it is possible to prevent the liquid surface in the vicinity of the rotating shaft from being dented and suppress foaming. As a result, a liquid flow from the radial direction toward the rotation axis is also formed on the lower surface side of the liquid flow regulation plate 5. This means that silver halide particles produced by continuously injecting an aqueous solution of silver salt and an aqueous solution of halogen salt as in the present invention and stirring and mixing are placed on the discharge flow of a stirring blade and dispersed in the colloidal aqueous solution in the reaction vessel. After that, in the growth process of the recycle type silver halide grains in which the aqueous solution of silver salt and the aqueous solution of halogen salt are again stirred and mixed by the liquid circulation in the reaction vessel, the recycling cycle is shortened and the inter-grain recycling is performed. The effect of reducing the difference in period and promoting uniform grain growth is obtained.
【０００８】一方、攪拌翼直下の回転軸付近についても
反応容器底面からの回転軸に沿った回転を伴った上方流
が観察される。２および２’は銀塩水溶液およびハロゲ
ン塩水溶液を連続的に注入するための注入ノズルであ
り、攪拌翼３に対向する方向に開口しているため、注入
された際は攪拌翼３に向かう流速成分を有するように設
けられている。該流速成分と前記の反応容器底面からの
回転軸に沿った回転を伴った上方流とが相乗されて、ノ
ズル２および２’より注入された銀塩水溶液およびハロ
ゲン塩水溶液は、保護コロイド水溶液により希釈される
と同時に、回転を伴った上方流により瞬時に混合され反
応しハロゲン化銀粒子が生成される。該ハロゲン化銀粒
子は攪拌翼に達した後、翼に対して水平遠心方向ないし
は斜め下方へ吐出され前述のリサイクル運動に至る。On the other hand, an upward flow accompanied by rotation along the rotation axis from the bottom of the reaction vessel is also observed near the rotation axis just below the stirring blade. Reference numerals 2 and 2 ′ are injection nozzles for continuously injecting the silver salt aqueous solution and the halogen salt aqueous solution, which are opened in a direction facing the stirring blade 3, and therefore, when injected, flow velocity toward the stirring blade 3 It is provided to have a component. The flow velocity component and the above-mentioned upward flow with rotation along the rotation axis from the bottom surface of the reaction vessel are synergistically combined so that the silver salt aqueous solution and the halogen salt aqueous solution injected from the nozzles 2 and 2 ′ are protected by the protective colloid aqueous solution. Simultaneously with the dilution, an upward flow accompanied by rotation instantaneously mixes and reacts to generate silver halide grains. After the silver halide grains reach the stirring blade, they are discharged in the horizontal centrifugal direction or obliquely downward with respect to the blade, and reach the above-described recycling motion.
【０００９】本実施例に示すような鉛直面に対し左右対
称形をした丸底形状の混合容器を使用して回転攪拌する
場合には、液が単調に回転するのみで相互に混じり合い
にくい現象を回避する方法として、図１に示すようなバ
ッフル板７を用いることは公知であり本発明においても
これを用いるものであるが、バッフル板を境界として回
転する液流の上流液面は凸となり下流液面は凹となるこ
とによって発泡が余儀なくされる。均一なハロゲン化銀
粒子を形成するに充分な回転速度を与えた場合、前記の
下流液面の凹状態は著しい空気混入現象を招き発泡を促
進させる。本発明においては図１に示す円筒４を攪拌翼
の周囲に設置することにより、発泡を抑制することがで
きた。すなわち攪拌翼で吐出された液の多く（使用する
攪拌翼の傾きにより変動はする）はまず円筒４の内側を
周回する流れとなり、そののち円筒４の下側および上側
より排出されるためバッフル板に対しては前記の空気混
入現象を招くほどの液面流速とはならない。In the case of using a round-bottomed mixing vessel having a symmetrical shape with respect to the vertical plane as shown in the present embodiment for rotational stirring, the liquids only rotate monotonously and are difficult to mix with each other. As a method for avoiding the above, it is known to use a baffle plate 7 as shown in FIG. 1 and this is also used in the present invention, but the upstream liquid surface of the liquid flow rotating with the baffle plate as a boundary becomes convex. Since the downstream liquid surface is concave, foaming is inevitable. When a rotation speed sufficient to form uniform silver halide grains is given, the concave state of the downstream liquid surface causes a remarkable air entrainment phenomenon and promotes foaming. In the present invention, foaming could be suppressed by installing the cylinder 4 shown in FIG. 1 around the stirring blade. That is, most of the liquid discharged by the stirring blade (which fluctuates depending on the inclination of the stirring blade used) first flows around the inside of the cylinder 4, and then is discharged from the lower side and the upper side of the cylinder 4, so that the baffle plate is discharged. However, the liquid surface velocity is not so high as to cause the above-mentioned air mixing phenomenon.
【００１０】ハロゲン化銀写真乳剤の製法においては攪
拌翼の吐出量の設定が重要な因子となるが、本発明にお
いては多くの実験を繰り返した結果、一般的なピッチド
タービン翼やピッチドパドル型攪拌翼を用いた場合、攪
拌翼の直径を混合容器の２０％ないし３０％として２０
０ｒｐｍ以上で６００ｒｐｍ以下好ましくは５００ｒｐ
ｍ以下の回転を与えて、前記の円筒の直径を攪拌翼の
１．１ないしは１．５倍にしたとき、希望するハロゲン
化銀粒子が得られ発泡も抑制することができた。本発明
はいわゆるダブルジェット法、コントロールドダブルジ
ェット法に適用する場合には、ハロゲン塩水溶液とと銀
塩水溶液の反応が迅速かつ完全に行われうるということ
から、銀塩水溶液とハロゲン塩水溶液の添加量をほぼ等
量に維持することによって、分散液（懸濁したハロゲン
化銀粒子を含む保護コロイド溶液）中の銀イオン濃度を
比較的容易に、あらかじめ設定した値に維持することが
可能でありハロゲン化銀写真乳剤製造上きわめて大きな
利点を有している。なお本発明において、支持棒６を反
応容器上方に設置した昇降装置（図示せず）により昇降
させることにより攪拌翼に対する円筒、液流規制板の相
対位置の微調整のほか、洗浄に対しても有効に作用する
ことは明らかであり、周知の技術で容易に実現可能であ
る。Although the setting of the discharge amount of the stirring blade is an important factor in the method for producing a silver halide photographic emulsion, many experiments were repeated in the present invention, and as a result, a general pitched turbine blade or pitched paddle type stirring was conducted. If a blade is used, the diameter of the stirring blade should be 20% to 30% of the mixing vessel.
0 rpm or more and 600 rpm or less, preferably 500 rp
When the rotation of m or less was applied to make the diameter of the cylinder 1.1 to 1.5 times that of the stirring blade, desired silver halide grains were obtained and foaming could be suppressed. When the present invention is applied to the so-called double jet method or controlled double jet method, the reaction between the aqueous solution of halogen salt and the aqueous solution of silver salt can be carried out rapidly and completely. By maintaining the addition amount at approximately the same amount, it is possible to maintain the silver ion concentration in the dispersion liquid (protective colloid solution containing suspended silver halide grains) at a preset value with relative ease. Yes, it has an extremely great advantage in producing a silver halide photographic emulsion. In the present invention, the support rod 6 is moved up and down by an elevating device (not shown) installed above the reaction container to finely adjust the relative positions of the cylinder and the liquid flow regulating plate with respect to the stirring blade, and also for cleaning. It is clear that it works effectively and can be easily realized by well-known techniques.
【００１１】[0011]
【実験例】以下本発明の効果を具体的な実験例により例
証する。[Experimental Example] The effect of the present invention will be illustrated below by a concrete experimental example.
【００１２】次の３種類の溶液を調製した。 溶液［Ａ］ ゼラチン １４．０ Ｋｇ ＮａＣｌ ２５０ ｇ 水を加えて ２４０．０Ｋｇに仕上げる 溶液［Ｂ］ ＮａＣｌ ２７．０ Ｋｇ 水を加えて ２５５．０Ｋｇに仕上げる 溶液［Ｃ］ ＡｇＮＯ３ ７０．０ Ｋｇ 水を加えて ２５５．０Ｋｇに仕上げる 製造装置は図１に示す。溶液［Ａ］は溶解設備（図示せ
ず）で溶解したあと反応容器（丸底円筒型：直径１１０
０ｍｍ）に満たしこれを４０゜Ｃに維持しながら、別の
容器で４０゜Ｃに保温した溶液［Ｂ］および［Ｃ］をそ
れぞれ別個にノズルより一定流量（５０００ｇ／ｍｉ
ｎ）で連続的に９０分間注入した。ノズルの位置は反応
容器中心軸対称としノズル開口部におけるノズル相互間
の距離を８０ｍｍとし、反応容器底面からノズル開口部
までの距離を１００ｍｍとした。なおノズルの内径はそ
れぞれ１４ｍｍとした。攪拌翼は直径３００ｍｍで４５
゜の傾きをもった翼の大きさ７５ｍｍ＊６０ｍｍのピッ
チドタービン翼を使用し４００ｒｐｍで攪拌した。攪拌
翼はその下端と反応容器底面との距離が１８０ｍｍの位
置に配置した。円筒は内径３７０ｍｍ深さ１５０ｍｍと
し攪拌翼と同心円上の位置で、円筒下端と反応容器底面
との距離が１５０ｍｍの位置に配置した。液流規制板
は、直径４００ｍｍの円板とし円筒の上端部より５０ｍ
ｍ隔てた位置に配置した。なお幅１１０ｍｍで反応容器
上端から底部近傍に至るまでの長さを有する板をバッフ
ル板として反応容器円周上に均等的に４箇所配置した。
一方比較実験−１として、上記の実験例の条件に対し円
筒と液流規制板を取り外した実験を、比較実験−２とし
て同じスケールで、前述の特公平２−６０１６６号公報
に示された装置でそれぞれ実験をおこなった。The following three types of solutions were prepared. Solution [A] Gelatin 14.0 Kg NaCl 250 g Add water to make 240.0 Kg Solution [B] NaCl 27.0 Kg Add water to make 255.0 Kg Solution [C] AgNO3 70.0 Kg Add water In addition, the manufacturing equipment for finishing to 255.0 Kg is shown in FIG. The solution [A] is dissolved in a dissolution facility (not shown) and then a reaction container (round-bottomed cylindrical type: diameter 110).
Solution (B) and [C] separately filled with 0 mm) and kept at 40 ° C in a separate container while being kept at 40 ° C separately from a nozzle at a constant flow rate (5000 g / mi).
n) was continuously infused for 90 minutes. The positions of the nozzles were symmetrical with respect to the central axis of the reaction vessel, the distance between the nozzles at the nozzle openings was 80 mm, and the distance from the bottom surface of the reaction vessel to the nozzle openings was 100 mm. The inner diameter of each nozzle was 14 mm. The stirring blade has a diameter of 300 mm and 45
A pitched turbine blade having a blade size of 75 mm * 60 mm with an inclination of ° was used and stirred at 400 rpm. The stirring blade was arranged at a position where the distance between the lower end of the stirring blade and the bottom surface of the reaction vessel was 180 mm. The cylinder had an inner diameter of 370 mm and a depth of 150 mm, and was arranged at a position concentric with the stirring blade, and at a position where the distance between the lower end of the cylinder and the bottom of the reaction vessel was 150 mm. The liquid flow control plate is a disc with a diameter of 400 mm and is 50 m from the upper end of the cylinder.
It was placed at a position separated by m. A plate having a width of 110 mm and a length from the upper end of the reaction container to the vicinity of the bottom was used as a baffle plate and was uniformly arranged at four positions on the circumference of the reaction container.
On the other hand, as Comparative Experiment-1, an experiment in which the cylinder and the liquid flow restricting plate were removed under the conditions of the above-mentioned Experimental Example was carried out as Comparative Experiment-2 on the same scale as the apparatus disclosed in Japanese Patent Publication No. 2-60166. I did each experiment.
【００１３】このようにして得られたハロゲン化銀粒子
を電子顕微鏡写真により平均粒径、標準偏差、および異
形粒子個数について測定した。その結果を表１に示す。The silver halide grains thus obtained were measured for their average grain size, standard deviation and number of irregularly shaped grains by electron micrograph. The results are shown in Table 1.
【表１】 [Table 1]
【００１４】比較実験における異形粒子は主として粗大
粒子であった。発泡の様子については、本発明の場合９
０分の混合時間終了直後において、液面より約８０ｍｍ
の発泡が認められた程度で後の水洗脱塩工程も支障なく
実施できたのに対し、比較実験−１においては液面より
５００ｍｍ以上の発泡が認められ、しかも液中への著し
い泡の混入が確認され、後の水洗脱塩工程を完全に実施
できなかった。比較実験−２においては液面より３００
ｍｍ以上の発泡が認められ、しかも液中への泡の混入は
比較実験−１より著しく、後の水洗脱塩工程を完全に実
施できなかった。The irregular-shaped particles in the comparative experiment were mainly coarse particles. Regarding the state of foaming, in the case of the present invention, 9
Immediately after the end of the mixing time of 0 minutes, approximately 80 mm from the liquid surface
Although the subsequent washing with water and desalting step could be carried out without any problem while the foaming was observed, in Comparative Experiment-1, foaming of 500 mm or more was recognized from the liquid surface, and a remarkable foaming in the liquid was observed. Contamination was confirmed, and the subsequent water washing desalination step could not be carried out completely. In Comparative Experiment-2, 300 from the liquid surface
Bubbling of mm or more was recognized, and the mixing of bubbles in the liquid was more remarkable than in Comparative Experiment-1, and the subsequent washing with water and desalting step could not be performed completely.
【００１５】以上の記載から明らかなように本発明によ
り次のような効果が得られる。 （１）従来より１桁上のオーダーとされる１０００リッ
トル以上の大量スケールでも発泡の問題もなくハロゲン
化銀異形粒子の発生を防止して均一な晶癖のハロゲン化
銀粒子を製造できるので大幅にコストダウンできるとと
もに、同一写真特性の乳剤を同時に大量に得ることがで
きる。 （２）粒径分布の狭いハロゲン化銀を生成できるので写
真特性の向上、特に省銀量化が可能となる。As is apparent from the above description, the present invention has the following effects. (1) Since it is possible to produce silver halide grains having a uniform crystal habit by preventing the generation of irregular silver halide grains even in a large scale of 1000 liters or more, which is on the order of one digit higher than before, and without the problem of foaming. The cost can be reduced, and a large amount of emulsions having the same photographic characteristics can be simultaneously obtained. (2) Since silver halide having a narrow grain size distribution can be produced, it is possible to improve photographic characteristics, especially to save silver.
【図１】本発明の一実施例の模式構成図FIG. 1 is a schematic configuration diagram of an embodiment of the present invention.
１ 反応容器 ２ ノズル ２’ノズル ３ 攪拌翼 ４ 円筒 ５ 液流規制板 ６ 支持棒 ７ バッフル板 DESCRIPTION OF SYMBOLS 1 Reaction container 2 Nozzle 2'Nozzle 3 Stirring blade 4 Cylinder 5 Liquid flow regulating plate 6 Support rod 7 Baffle plate
Claims (2)
子製造装置において、反応容器中に、翼の遠心方向ない
し斜め下方に液流を生ぜしめる攪拌翼と、その周囲に固
定された前記攪拌翼径の１．１ないし１．５倍の直径を
有する円筒と、該円筒の上端部より離れた位置に配置さ
れ攪拌翼回転軸下方向の液流を規制し液面からの空気混
入を抑制する前記円筒とほぼ同径の液流規制板と、前記
攪拌翼の下方に位置し上方にハロゲン塩水溶液および銀
塩水溶液を吐出する注入ノズルとから成ることを特徴と
するハロゲン化銀写真乳剤の製造装置。1. An apparatus for producing silver halide grains by the double jet method, comprising: a stirring blade for generating a liquid flow in a reaction vessel in a centrifugal direction or obliquely downward of the blade; and a stirring blade diameter fixed around the stirring blade. A cylinder having a diameter of 1.1 to 1.5 times, and a cylinder arranged at a position separated from an upper end of the cylinder to restrict a liquid flow in a downward direction of a rotation axis of a stirring blade and suppress air inclusion from a liquid surface. An apparatus for producing a silver halide photographic emulsion, comprising a liquid flow control plate having a diameter substantially the same as that of the above, and an injection nozzle located below the stirring blade and discharging an aqueous solution of halogen salt and an aqueous solution of silver salt upward.
いし３０％とした請求項１記載のハロゲン化銀写真乳剤
製造装置。2. A silver halide photographic emulsion manufacturing apparatus according to claim 1, wherein the diameter of the stirring blade is 20% to 30% of the diameter of the reaction vessel.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3294941A JP2624589B2 (en) | 1991-10-14 | 1991-10-14 | Equipment for manufacturing silver halide photographic emulsions |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3294941A JP2624589B2 (en) | 1991-10-14 | 1991-10-14 | Equipment for manufacturing silver halide photographic emulsions |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH05107668A true JPH05107668A (en) | 1993-04-30 |
| JP2624589B2 JP2624589B2 (en) | 1997-06-25 |
Family
ID=17814262
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP3294941A Expired - Lifetime JP2624589B2 (en) | 1991-10-14 | 1991-10-14 | Equipment for manufacturing silver halide photographic emulsions |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2624589B2 (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005296894A (en) * | 2004-04-15 | 2005-10-27 | Satake Chemical Equipment Mfg Ltd | Stirring blade |
| CN105597582A (en) * | 2016-03-24 | 2016-05-25 | 华东理工大学 | Mechanically-stirring type continuous emulsifier and emulsifying method |
| CN105664745A (en) * | 2016-03-24 | 2016-06-15 | 华东理工大学 | Delivery reinforced mechanical stirring type continuous emulsifier and emulsifying method |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02262640A (en) * | 1989-04-03 | 1990-10-25 | Konica Corp | Apparatus for producing silver halide emulsion |
-
1991
- 1991-10-14 JP JP3294941A patent/JP2624589B2/en not_active Expired - Lifetime
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02262640A (en) * | 1989-04-03 | 1990-10-25 | Konica Corp | Apparatus for producing silver halide emulsion |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005296894A (en) * | 2004-04-15 | 2005-10-27 | Satake Chemical Equipment Mfg Ltd | Stirring blade |
| CN105597582A (en) * | 2016-03-24 | 2016-05-25 | 华东理工大学 | Mechanically-stirring type continuous emulsifier and emulsifying method |
| CN105664745A (en) * | 2016-03-24 | 2016-06-15 | 华东理工大学 | Delivery reinforced mechanical stirring type continuous emulsifier and emulsifying method |
| CN105597582B (en) * | 2016-03-24 | 2019-07-02 | 华东理工大学 | A kind of mechanical agitation type Continuous Emulsifier and emulsification method |
| CN105664745B (en) * | 2016-03-24 | 2019-07-02 | 华东理工大学 | It is a kind of to strengthen the mechanical agitation type Continuous Emulsifier conveyed and emulsification method |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2624589B2 (en) | 1997-06-25 |
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