JPS60201333A - Apparatus for producing silver halide photographic emulsion - Google Patents

Apparatus for producing silver halide photographic emulsion

Info

Publication number
JPS60201333A
JPS60201333A JP59059200A JP5920084A JPS60201333A JP S60201333 A JPS60201333 A JP S60201333A JP 59059200 A JP59059200 A JP 59059200A JP 5920084 A JP5920084 A JP 5920084A JP S60201333 A JPS60201333 A JP S60201333A
Authority
JP
Japan
Prior art keywords
mixer
path
silver halide
stirring blade
conduit
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
Application number
JP59059200A
Other languages
Japanese (ja)
Other versions
JPH0254932B2 (en
Inventor
Nobuo Saito
斎藤 延夫
Tsutomu Sawada
沢田 務
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Mitsubishi Paper Mills Ltd
Original Assignee
Mitsubishi Paper Mills Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Mitsubishi Paper Mills Ltd filed Critical Mitsubishi Paper Mills Ltd
Priority to JP59059200A priority Critical patent/JPS60201333A/en
Publication of JPS60201333A publication Critical patent/JPS60201333A/en
Publication of JPH0254932B2 publication Critical patent/JPH0254932B2/ja
Granted legal-status Critical Current

Links

Classifications

    • GPHYSICS
    • G03PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
    • G03CPHOTOSENSITIVE MATERIALS FOR PHOTOGRAPHIC PURPOSES; PHOTOGRAPHIC PROCESSES, e.g. CINE, X-RAY, COLOUR, STEREO-PHOTOGRAPHIC PROCESSES; AUXILIARY PROCESSES IN PHOTOGRAPHY
    • G03C1/00Photosensitive materials
    • G03C1/005Silver halide emulsions; Preparation thereof; Physical treatment thereof; Incorporation of additives therein
    • G03C1/015Apparatus or processes for the preparation of emulsions
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01FMIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F27/00Mixers with rotary stirring devices in fixed receptacles; Kneaders
    • B01F27/80Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis
    • B01F27/91Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis with propellers
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01FMIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F27/00Mixers with rotary stirring devices in fixed receptacles; Kneaders
    • B01F27/05Stirrers
    • B01F27/11Stirrers characterised by the configuration of the stirrers
    • B01F27/15Stirrers with tubes for guiding the material
    • GPHYSICS
    • G03PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
    • G03CPHOTOSENSITIVE MATERIALS FOR PHOTOGRAPHIC PURPOSES; PHOTOGRAPHIC PROCESSES, e.g. CINE, X-RAY, COLOUR, STEREO-PHOTOGRAPHIC PROCESSES; AUXILIARY PROCESSES IN PHOTOGRAPHY
    • G03C2200/00Details
    • G03C2200/09Apparatus

Abstract

PURPOSE:To obtain silver halide particles having a narrow grain size distribution and a uniform particle crystal habit by increasing continuously the cross sectional area of a conduit path toward the upper aperture of the conduit path thereby adding a circular flow component to the discharged liquid flow. CONSTITUTION:A mixer 2 has an aperture having a circular cross section at the bottom end 21 of a cylindrical casing and has a conduit path 6 opening only in the direction of an impeller revolving shaft 6 at the top end of the cylindrical casing. The path 6 has the length in the direction of the shaft 5 enough to convert the discharge flow to vertical flow. The length of the conduit path is in a >=0.01 range in terms of the ratio of the length value of the conduit path with respect to the area value of the aperture of the conduit path. The path 6 has a circular cross section in the lower aperture 61 and the cross sectional area increases continuously from an intermediate point (b) toward the center of the adjacent conduit path so that said path is made into the type combined with the semielliptical cross section in an upper aperture 62. The increase and continuous change in the area of the upper aperture of the conduit path from the area in the lower aperture provide the peripheral component of the impeller revolving shaft to the vertical flow discharged from the path 6 according to the discharge from the path 6 or the inside volume of the mixer 2.

Description

【発明の詳細な説明】 本発明はハロゲン化銀写真乳剤の製造装置に関し、更に
詳細には多量製造の場合にも粒径分布が狭く粒子晶癖の
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
ン化銀写真乳剤の製造装置に関するものである。
DETAILED DESCRIPTION OF THE INVENTION The present invention relates to an apparatus for producing a silver halide photographic emulsion, and more specifically, it is capable of producing silver halide grains with a narrow grain size distribution and uniform grain crystal habit even in the case of mass production. This invention relates to an apparatus for producing silver halide photographic emulsions.

粒径分布の狭い均一晶癖の7・ロゲン化銀写真乳剤の製
造装置として、米国特許第3,145,650号明細書
、英国特許第1,323,464号明細書、米国特許第
3,694283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。
As an apparatus for producing a silver halide photographic emulsion having a homogeneous crystal habit with a narrow grain size distribution, U.S. Pat. Techniques disclosed in Japanese Patent Publication No. 694283, Japanese Patent Publication No. 55-10545, etc. are known.

これらの装置は、水溶性根塩及び水溶性ハロゲン塩の均
一な反応条件を生みだすために、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発明され混合
器の形状、攪拌装置の形状、ハロゲン塩水溶液および銀
塩水溶液の供給方式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径分布
が狭く、粒子晶癖の均一なノ・ロゲン化銀粒子を製造す
ることは困難である。
These devices were invented to create uniform reaction conditions for water-soluble root salts and water-soluble halogen salts, and to simplify the manufacturing process of silver halide photographic emulsions. The shape, the supply method of the halogen salt aqueous solution and the silver salt aqueous solution, etc. have been improved. However, with these techniques, it is difficult to produce silver halogenide grains with sufficiently narrow grain size distribution and uniform grain crystal habit due to drawbacks such as lack of uniformity in the circulation flow of the liquid throughout the reaction vessel. be.

一方、特開昭57−92524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法主体の流れに変換すること
によって改善するノ・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
性は末だ充分ではなく、粒径分布の充分に狭いノ・ロゲ
ン化銀粒子を製造することができなかった。
On the other hand, Japanese Patent Application Laid-open No. 57-92524 discloses a method for improving the uniformity of the circulation flow of liquid throughout the reaction vessel by converting the discharge flow from a stirring blade into a mainly vertical flow using a liquid flow regulating plate. - An apparatus for producing a silver halogenide emulsion is disclosed. However, even with this technique, the circulation of the liquid was still insufficient, and silver halogenide grains with a sufficiently narrow particle size distribution could not be produced.

本発明者等は従来技術を改良し、粒径分布が狭く、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の製造装置について実開昭59−
3921に開示した。
The present inventors improved the conventional technology and developed a silver halide photographic emulsion manufacturing apparatus capable of manufacturing silver halide grains having a narrow grain size distribution and uniform grain crystal habit.
3921.

かかる技術にもとずくノ・ロゲン化銀写真乳剤の製造装
置を第1図、第2図・、および第3図に示す。
An apparatus for producing a silver halogenide photographic emulsion based on this technique is shown in FIGS. 1, 2, and 3.

保護コロイド水溶液が満たされている反応容器1中にそ
の内部に該保護コロイド水溶液が満たされる如く設けら
れた混合器2を有し、該混合器にその下端部開放端21
からハロゲン塩水溶液と銀塩水溶液とを供給管3.3′
を通じて別々に供給し、該両反応液を混合器2中の保護
コロイド水溶液により各々稀釈し、nif記混合器2に
設けられた攪拌翼4によって両反応液を急激に欅拌混合
して反応せしめ、ハロゲン化銀粒子を生成させ、ただち
に導通路6を通して、前記混合器2外上方の反応容器中
の保護コロイド水溶液の中に排出させる。混合器2から
排出される吐出循環流は導通路6より均一な鉛直流とさ
れ反応容器混合器循環性が向上し個々のハロゲン化銀粒
子の成長プロセスが均一化されることによって粒径分布
の狭いハロゲン化銀粒子を製造するものである。
A reaction vessel 1 filled with a protective colloid aqueous solution has a mixer 2 installed so that the inside thereof is filled with the protective colloid aqueous solution, and the mixer has a lower open end 21.
The halogen salt aqueous solution and silver salt aqueous solution are supplied from pipe 3.3'.
Both reaction solutions are diluted with a protective colloid aqueous solution in the mixer 2, and both reaction solutions are rapidly stirred and mixed by the stirring blade 4 provided in the mixer 2 to react. , silver halide grains are produced and immediately discharged through the conduit 6 into the protective colloid aqueous solution in the reaction vessel above the outside of the mixer 2. The discharge circulating flow discharged from the mixer 2 is made into a uniform vertical flow through the conduit 6, improving the circulation of the reaction vessel mixer and making the growth process of individual silver halide grains uniform, thereby improving the grain size distribution. It produces narrow silver halide grains.

本発明者等はかかる技術にもとづき、よ昨粒径分布の狭
いハロゲン化銀粒子の製造装置、多量のハロゲン化銀粒
子の製造に適した製造装置について鋭意検討を続けたと
ころ、かかる技術においてより粒径分布の狭いハロゲン
化銀粒子は混合器内攪拌翼回転数をたかめ、混合器導通
路よりの吐出量を増加させることによって達成できるこ
とが明らかとなった。
Based on this technology, the present inventors have continued to conduct intensive studies on production equipment for silver halide grains with a narrower grain size distribution and production equipment suitable for production of large quantities of silver halide grains, and have found that with this technology, It has become clear that silver halide particles with a narrow particle size distribution can be achieved by increasing the rotational speed of the stirring blade in the mixer and increasing the amount of discharge from the mixer conduit.

しかしながら、混合器導通路よりの吐出量を増加させる
と、一般にはま1<麹型結晶と呼ばれる結晶内にただ1
個の双晶面を有し、分散媒体との境界面が(1,0,0
)面、(1,1,1)面またはこれらの混合した而から
成るノ・ロゲン化銀結晶の異形粒子が発生し、均一なl
・ロゲン化銀粒子晶゛癖が得られないとわう問題が判明
した。
However, when the discharge amount from the mixer conduit is increased, generally speaking, there is only 1 in the crystal called koji-type crystal.
The interface with the dispersion medium is (1,0,0
) planes, (1,1,1) planes, or a mixture of these planes.
・It was discovered that the problem was that silver halide grain crystal habit could not be obtained.

本発明の目的は、前記第1図、第2図も・よび第3図に
示される技術を改良し、より粒径分布が狭く粒子晶癖の
均一なノ・ロゲン化銀粒子を製造することができる/・
ロゲン化銀写真乳剤の製造装置を提供することにある。
The purpose of the present invention is to improve the techniques shown in FIGS. 1, 2, and 3, and to produce silver halogenide grains with a narrower grain size distribution and uniform grain crystal habit. can/・
An object of the present invention is to provide an apparatus for producing a silver halide photographic emulsion.

本発明の他の目的はノ・ロゲン化銀粒子の多3%i%Q
造を容易ならしめるI・ロゲン化銀写典乳剤の製造装置
を提供することにある。
Another object of the present invention is to obtain a silver halogenide grain containing 3%i%Q.
An object of the present invention is to provide an apparatus for producing an I.silver halide manuscript emulsion that facilitates production.

本発明の上記目的は、反応容器中に攪拌翼とその周囲に
固定されたケーシングからなる混合器を有し、該ケーシ
ングは下端部にノ・ロゲン塩水溶液、銀塩水溶液、およ
び保護コロイド水溶液を該混合器に導入する開口部を有
し、上端部に該混合器にて生成された・・ロゲン化銀粒
子を排出する開口部を有し、該上端部開口部は排出され
る液流が攪拌翼回転軸方向の鉛直流となるに充分な攪拌
翼回転軸方向長さをもち攪拌翼回転軸方向に開口する複
数の導通路よりなるノ・ロゲン化銀写真乳剤の製造装置
において、該導通路横断面積を該導通路上方開口部に向
けて連続的に増加させて該導通路より排出される液流に
円周流成分を付加させたI・ロゲン化銀写真乳剤の製造
装置によって達成される。
The above object of the present invention is to have a mixer consisting of a stirring blade and a casing fixed around the stirring blade in a reaction vessel, and the casing has a lower end containing an aqueous solution of a nitrogen salt, an aqueous silver salt solution, and an aqueous protective colloid solution. It has an opening for introducing into the mixer, and an opening for discharging the silver halide particles generated in the mixer at the upper end, and the upper end opening allows the discharged liquid stream to flow through the mixer. In an apparatus for producing a silver halogenide photographic emulsion, which comprises a plurality of conductive passages opening in the direction of the stirring blade rotation axis and having a sufficient length in the rotation axis direction of the stirring blade to generate a vertical flow in the direction of the rotation axis of the stirring blade, This is achieved by an apparatus for producing an I silver halide photographic emulsion, in which the cross-sectional area of the passage is continuously increased toward the upper opening of the passage, and a circumferential flow component is added to the liquid flow discharged from the passage. Ru.

以下、添付図面にもとすき本発明の実施態様C千あり、
第4図は混合器2の上端部平面図であり、第5図は混合
器2の第4図a−mに沿った拡大縦断面図である。
Hereinafter, there are several embodiments of the present invention shown in the accompanying drawings.
4 is a plan view of the upper end of the mixer 2, and FIG. 5 is an enlarged longitudinal cross-sectional view of the mixer 2 along the line 4a-m.

ハロゲン塩水溶液と銀塩水溶液はそれぞれ供給管3,3
′を通して反応容器1内に設けられた混合器2の下端部
へ連続的に供給される。
The halogen salt aqueous solution and silver salt aqueous solution are supplied to supply pipes 3 and 3, respectively.
' is continuously supplied to the lower end of the mixer 2 provided in the reaction vessel 1.

反応容器1には保護コロイド水溶液が満たされており、
混合器2は該保護コロイド水溶液の液面下に設けられ、
混合器2内部は該保護コロイド水溶液によって満たされ
る。反応容器1小の保護コロイド水溶液は該混合器2の
作用により、該混合器2内を下方から上方へ横切るよう
に常に対流せしめられる。
The reaction vessel 1 is filled with a protective colloid aqueous solution,
The mixer 2 is provided below the surface of the protective colloid aqueous solution,
The inside of the mixer 2 is filled with the protective colloid aqueous solution. The protective colloid aqueous solution in the reaction vessel 1 is constantly caused to convect by the action of the mixer 2 so as to cross the inside of the mixer 2 from the bottom to the top.

混合器2は円筒形ケーシング下端部21に横断面円形の
開口部を有しており、前記円筒形ケーシング上端部に攪
拌翼回転軸5方向にのみ開口する導通路6を有している
。導通路6は吐出流を鉛直流にするための充分な攪拌翼
回転軸5方向長さを有している。導通路長さは装置の諸
元によって変化するものであるが、導通路開口部面積値
に対する導通路長値の比として0.01以上の範囲にあ
るのが好まし−。導通路6はその下方開口部61におい
ては横断面円形であるが、中間地点すより連続的に隣接
する導通路中心方向に横断面積が拡大し、その上方開口
部62においては横断面半楕円結合形である。導通路6
の上方開口部面積の下方開口部面積よりの増加量ふ・よ
び連続的変化敏は一概に決定できるものではなく、導通
路6からの吐出量あるいは混合器2の内容積に応じて導
通路6から排出される鉛直流に攪拌翼回転軸円周方向成
分を付加する構成であればよい。
The mixer 2 has an opening with a circular cross section at the lower end 21 of a cylindrical casing, and has a conduction path 6 that opens only in the direction of the stirring blade rotating shaft 5 at the upper end of the cylindrical casing. The conduit 6 has a sufficient length in the direction of the stirring blade rotation axis 5 to make the discharge flow vertical. Although the length of the conductive path varies depending on the specifications of the device, it is preferable that the ratio of the length of the conductive path to the area of the opening of the conductive path is in a range of 0.01 or more. The conductive path 6 has a circular cross section at its lower opening 61, but the cross sectional area continuously expands from the intermediate point toward the center of the adjacent conductive path, and at its upper opening 62, the cross section becomes a semi-elliptical joint. It is the shape. Conduction path 6
The amount of increase in the area of the upper opening from the area of the lower opening and the continuous change sensitivity cannot be determined unconditionally; Any configuration may be used as long as it adds a component in the circumferential direction of the rotation axis of the stirring blade to the vertical flow discharged from the stirring blade.

混合器2には鉛直方向の回転軸5に取付けられノぐ たピッチド4ドル型攪拌翼4が設けられている。The mixer 2 has a nozzle attached to a vertical rotating shaft 5. A pitched four dollar type stirring blade 4 is provided.

攪拌翼4は供給管3,3′を通して円筒形ケーシング下
端部21の開口部に供給される両反応液が混合器2中の
保護コロイド水溶液により稀釈されたのち、この両反応
液を急激に攪拌混合せしめ、ハロゲン化銀粒子を生成さ
せるとともに、生成したハロゲン化銀粒子を直ちに混合
器2外上方に導通路6から反応容器1中の保護コロイド
水溶液を排出せしめるものである。
The stirring blade 4 rapidly stirs both reaction liquids supplied to the opening of the lower end 21 of the cylindrical casing through the supply pipes 3 and 3' after the reaction liquids are diluted with the protective colloid aqueous solution in the mixer 2. The aqueous protective colloid solution in the reaction vessel 1 is mixed to produce silver halide particles, and the aqueous protective colloid solution in the reaction vessel 1 is immediately discharged from the conduit 6 to the outside and above of the mixer 2.

本発明に用いられるハロゲン化銀写真乳剤の製造装置は
第1図、第4図および第5図に示す構成のものに限定さ
れることな(特許請求の範囲に記載された範囲内で種々
の変更が可能であることは言うまでもない。
The apparatus for producing the silver halide photographic emulsion used in the present invention is not limited to the configuration shown in FIGS. 1, 4, and 5. Needless to say, changes are possible.

又、本発明に謄いて混合器2上方の保護コロイド水溶液
表面直下に流動制御板を使用することは、導通路6から
排出される吐出循環流量を発泡を伴なわずに増加させる
ことができるので有利に利用である。
Further, by using a flow control plate directly below the surface of the protective colloid aqueous solution above the mixer 2 according to the present invention, the discharge circulation flow rate discharged from the conduit passage 6 can be increased without causing foaming. Use it to your advantage.

本発明は、混合器内で生成したI・ロゲン化銀粒子を攪
拌翼の吐出流にのせて混合器外へ排出させた後、反応容
器内を循環させ、再び混合器へ1ノサイクルさせる。こ
のリサイクル運動の繰り返しのし、かつ粒子間の周期差
を少なくするべ(、混合器導通路よりの吐出量を増大さ
せた時に、混合器内の循環流滞留時間の減少によって発
生する〕・ロゲン化銀異形粒子の発生を混合器内容積を
拡大することなく、導通路より排出される均一な鉛直流
に混合器内での攪拌混合を補完するため円周流成分を付
加させる構成をもつ導通路上方開口部を有するハロゲン
化銀写真乳剤の製造装置によって実現したものである。
In the present invention, the I silver halide particles produced in the mixer are discharged from the mixer by being carried by the discharge stream of the stirring blade, and then circulated in the reaction vessel and returned to the mixer for one cycle. It is necessary to repeat this recycling movement and reduce the period difference between particles (which occurs due to a decrease in the residence time of the circulation flow in the mixer when the discharge amount from the mixer conduit is increased). A conductor with a configuration that adds a circumferential flow component to the uniform vertical flow discharged from the conductor passage to supplement the stirring and mixing within the mixer, without increasing the internal volume of the mixer to prevent the generation of irregularly shaped silver oxide particles. This was realized by a silver halide photographic emulsion manufacturing apparatus having an opening on the road side.

本発明は、いわゆるシングルジz7ト法、ダブルジェッ
ト法、コントロールタフルジェット法に適用する場合に
は、混合器における反応が迅速かつ完全に行なわれうる
ということから、銀塩水溶液とハロゲン塩水溶液との添
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/・ロゲン化銀粒子を含む保護コロイド水溶液)中の
銀イオン濃度を比較的容抹に予め設定した値に維持する
ことが可能であり、ノ・ロゲン化銀写真乳剤製造上極め
で大きな利点を有している。
When the present invention is applied to the so-called single jet method, double jet method, and controlled jet method, the reaction in the mixer can be carried out quickly and completely. The silver ion concentration in the dispersion (protective colloid aqueous solution containing suspended silver halide particles) is maintained at a relatively constant preset value by maintaining approximately the same amount of silver ion. This method is extremely advantageous in the production of silver halogenide photographic emulsions.

以下、本発明の効果を具体的な実施例により例証する。Hereinafter, the effects of the present invention will be illustrated by specific examples.

実施例 次の3種類の溶液を調整した。Example The following three types of solutions were prepared.

製造装置としては第1図第4図ふ・よび第5図に示す構
成のものを用いた。すなわち、溶液[A)を半球底円翰
形反応容器(直径400−)に満たし、溶液CB)およ
び〔C〕を管3,3′をi!flして反応温度60℃で
60分間にわたって定速(167cc/朋)で別々に且
つ連続的に添加した。
The manufacturing apparatus used was one having the configuration shown in FIG. 1, FIG. 4, and FIG. 5. That is, a hemispherical bottom conical reaction vessel (diameter 400-) is filled with solution [A), and solutions CB) and [C] are poured into tubes 3 and 3' i! fl were added separately and continuously at a constant rate (167 cc/home) over 60 minutes at a reaction temperature of 60°C.

混合器はケーシングが直径80−高さ70−+7)円筒
形で、下端部21は直径30−で開口しており、上端部
導通路6は下方開口部61の直径25鶴円形で鉛直方向
に20鰭の長さであり、E方間ロ部62下5鴎の地点す
より連続的に隣接する導通路中心方向に横断面積が増加
し、上方開口部62は長直径30−短直径25難の半楕
円結合形である。
The mixer has a cylindrical casing with a diameter of 80 mm and a height of 70 mm. It has a length of 20 fins, and the cross-sectional area increases in the direction of the center of the conduit passage that is continuously adjacent to the lower part 62 of the E side, and the upper opening 62 has a long diameter of 30 - short diameter of 25 fins. It is a semi-elliptic combination of.

攪拌R4は翼長20−の角度45°ピツチドパドルを用
い、回転数150Or、p、mで回転させた。
Stirring R4 was performed using a pitched paddle having a blade length of 20 degrees and an angle of 45 degrees, and was rotated at a rotation speed of 150 Or, p, and m.

一方、上記本発明の実施例において導通路断面積を一定
にして上方開口部62を直径25態円形とした場合につ
いて比較実験を行なった。
On the other hand, a comparative experiment was conducted in the case where the cross-sectional area of the conductive path was constant and the upper opening 62 was made circular with a diameter of 25 in the above embodiment of the present invention.

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。その結果は表−1の通りであった。
The silver halide grains thus obtained were measured for average grain size, standard deviation, and number of irregularly shaped grains using electron micrographs. The results were as shown in Table-1.

比較実験におけるハロゲン化銀粒子の大部分は(1,0
,0)面を有する結晶であったが異形粒子ははまぐり型
結晶であった。
Most of the silver halide grains in comparative experiments were (1,0
, 0), but the irregularly shaped particles were clam-shaped crystals.

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。
As is clear from the above description, the following effects can be obtained by the present invention.

(1)混合器導通路上方開口部面積を下方開口部面積よ
り拡大させた導通路を使用することにより混合器より排
出される鉛直流に円周流成分を付加することによゆ、混
合器内での攪拌混合を補完しハロゲン化銀異形粒子の発
生を防止して粒径分布が狭く、均一晶癖のハロゲン化銀
写真乳剤が製造できる。
(1) By adding a circumferential flow component to the vertical flow discharged from the mixer by using a conduit passage whose upper opening area is larger than the lower opening area, the mixer It is possible to produce a silver halide photographic emulsion with a narrow grain size distribution and a uniform crystal habit by supplementing the stirring and mixing in the process and preventing the generation of irregularly shaped silver halide grains.

し)混合器よりの吐出循環流量を増加させられることに
より、多量スケールでの循環性低下の問題が解消され多
量のノ・ロゲン化銀写真乳剤を製造することが可能とな
る。
(b) By increasing the circulating flow rate discharged from the mixer, the problem of poor circulation on a large scale is solved, and it becomes possible to produce a large amount of silver halogen photographic emulsion.

(3)粒径分布の狭い、均一晶癖な・・ロゲン化集が製
造できるので写真性能の向上、とくに省銀量化が可能と
なる。
(3) Since it is possible to produce a halogenated agglomerate with a narrow particle size distribution and a uniform crystal habit, it is possible to improve photographic performance, and in particular to save silver.

【図面の簡単な説明】[Brief explanation of drawings]

第1図は従来の技術にもとすく、および本発明による装
置の概略縦断面図、第2図り従来技術にもとず(混合器
部分の拡大縦断面図、第3図は第2図の平面図、第4図
は本発明による装置の混合器部分の拡大平面図、第5図
線本発明による装置の混合器部分箱4因am線に沿った
拡大縦断面図である。 図中、1は反応容器、2は混合器、21U下端開放端、
3.3′は反応液供給管、4は攪拌翼、5は攪拌翼回転
軸、6は導通路、61は導通路下方開口部、62は導通
路上方開口部を示す。 第11!1 第2図第3図 第4図 q 第5rJ4
FIG. 1 is a schematic longitudinal cross-sectional view of a device according to the present invention based on the prior art; FIG. 2 is an enlarged longitudinal cross-sectional view of a mixer portion; 4 is an enlarged plan view of the mixer portion of the device according to the present invention, and FIG. 5 is an enlarged longitudinal cross-sectional view of the mixer portion box of the device according to the present invention taken along line 4. In the figure, 1 is a reaction container, 2 is a mixer, 21U lower open end,
3.3' is a reaction liquid supply pipe, 4 is a stirring blade, 5 is a stirring blade rotating shaft, 6 is a conduit passage, 61 is a lower opening of the conduit passage, and 62 is an upper opening of the conduit passage. 11!1 Figure 2 Figure 3 Figure 4 q 5rJ4

Claims (1)

【特許請求の範囲】 反応容器中に、攪拌翼とその周囲に固定されたケーシン
グからなる混合器を有し、該ケーシングは下端部にハロ
ゲン塩水溶液、銀塩水溶液および保護コロイド水溶液を
該混合器に導入する開口部を有し、上端部に該混合器に
て生成されたハロゲン化銀粒子を排出する開口部を有し
、該上端部開口部は排出される液流が攪拌翼回転軸方向
の鉛直流となるに充分な攪拌翼回転軸方向長さをもち。 攪拌翼回転軸方向に開口する複数の導通路よりなるハロ
ゲン化銀写真乳剤の製造装置において、該導通路横断面
積を該導通路上方開口部に向けて連続的に増加させて該
導通路より排出される液流に円周流成分を付加させたこ
とを特徴とするハロゲン化銀写真乳剤の製造装置。
[Scope of Claims] A mixer consisting of a stirring blade and a casing fixed around the stirring blade is provided in the reaction vessel, and the casing has a lower end containing a halogen salt aqueous solution, a silver salt aqueous solution, and a protective colloid aqueous solution into the mixer. The upper end has an opening for introducing the silver halide particles generated in the mixer, and the upper end has an opening for discharging the silver halide particles generated in the mixer, and the upper end opening allows the liquid flow to be discharged in the direction of the rotation axis of the stirring blade. The stirring blade has a sufficient length in the axial direction to produce a vertical flow. In a silver halide photographic emulsion production apparatus comprising a plurality of conductive passages opening in the direction of the rotating axis of the stirring blade, the cross-sectional area of the conductive passage is continuously increased toward the upper opening of the conductive passage and discharged from the conductive passage. 1. A silver halide photographic emulsion production apparatus characterized in that a circumferential flow component is added to a liquid flow.
JP59059200A 1984-03-26 1984-03-26 Apparatus for producing silver halide photographic emulsion Granted JPS60201333A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP59059200A JPS60201333A (en) 1984-03-26 1984-03-26 Apparatus for producing silver halide photographic emulsion

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP59059200A JPS60201333A (en) 1984-03-26 1984-03-26 Apparatus for producing silver halide photographic emulsion

Publications (2)

Publication Number Publication Date
JPS60201333A true JPS60201333A (en) 1985-10-11
JPH0254932B2 JPH0254932B2 (en) 1990-11-26

Family

ID=13106543

Family Applications (1)

Application Number Title Priority Date Filing Date
JP59059200A Granted JPS60201333A (en) 1984-03-26 1984-03-26 Apparatus for producing silver halide photographic emulsion

Country Status (1)

Country Link
JP (1) JPS60201333A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS62106451A (en) * 1985-11-02 1987-05-16 Konishiroku Photo Ind Co Ltd Production of photographic silver halide emulsion

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS62106451A (en) * 1985-11-02 1987-05-16 Konishiroku Photo Ind Co Ltd Production of photographic silver halide emulsion

Also Published As

Publication number Publication date
JPH0254932B2 (en) 1990-11-26

Similar Documents

Publication Publication Date Title
US6422736B1 (en) Scalable impeller apparatus for preparing silver halide grains
US4251627A (en) Jet mixing in preparation of monodisperse silver halide emulsions
US3897935A (en) Apparatus for the preparation of a photographic emulsion
US4147551A (en) Process for photographic emulsion precipitation in a recycle stream
CA1115585A (en) Method and apparatus suitable for the preparation of agx-emulsions
PL131793B1 (en) Gas dissipating rotary apparatus,especially for treatment of molten metal bath
JPS5858288B2 (en) Method and apparatus for producing silver halide grains
JPS5926129A (en) Apparatus for preparing dispersion liquid droplets
US5096690A (en) Method and apparatus for manufacturing silver halide grains
JP3165923B2 (en) Method for producing poorly water-soluble salt crystal particles and apparatus for producing the same
US6443611B1 (en) Apparatus for manufacturing photographic emulsions
US5213772A (en) Apparatus for forming silver halide grains
JPH08332364A (en) Solution mixing device
JPS5858289B2 (en) Method and apparatus for producing silver halide grains
JPS60201333A (en) Apparatus for producing silver halide photographic emulsion
JPH02167818A (en) Production of silver halide particle
US3705034A (en) Process and apparatus for producing improved photographic emulsion
JPH0128084B2 (en)
EP0729062B1 (en) Sonic micro reaction zones in silver halide emulsion precipitation process
US3628959A (en) Process for the preparation of photographic emulsion
JPH0320829Y2 (en)
JPS6389837A (en) Apparatus for producing photographic silver halide emulsion
CN207828161U (en) titanium dioxide coating system
JP3575642B2 (en) Method and apparatus for producing silver halide emulsion
GB1504185A (en) Apparatus for cooling aerating and circulating a liquid medium within a reactor