JPS6389837A - Apparatus for producing photographic silver halide emulsion - Google Patents
Apparatus for producing photographic silver halide emulsionInfo
- Publication number
- JPS6389837A JPS6389837A JP61236721A JP23672186A JPS6389837A JP S6389837 A JPS6389837 A JP S6389837A JP 61236721 A JP61236721 A JP 61236721A JP 23672186 A JP23672186 A JP 23672186A JP S6389837 A JPS6389837 A JP S6389837A
- Authority
- JP
- Japan
- Prior art keywords
- mixer
- silver halide
- aqueous solution
- soln
- silver
- 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
- -1 silver halide Chemical class 0.000 title claims abstract description 56
- 239000004332 silver Substances 0.000 title claims abstract description 49
- 229910052709 silver Inorganic materials 0.000 title claims abstract description 49
- 239000000839 emulsion Substances 0.000 title claims description 21
- 238000003756 stirring Methods 0.000 claims abstract description 23
- 239000002245 particle Substances 0.000 claims abstract description 20
- 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 claims abstract description 16
- 230000001681 protective effect Effects 0.000 claims abstract description 14
- 239000007864 aqueous solution Substances 0.000 claims description 29
- 238000004519 manufacturing process Methods 0.000 claims description 16
- 239000000084 colloidal system Substances 0.000 claims description 13
- 229910052736 halogen Inorganic materials 0.000 claims description 11
- 239000007788 liquid Substances 0.000 claims description 6
- 238000007599 discharging Methods 0.000 claims description 2
- 239000013078 crystal Substances 0.000 abstract description 9
- 150000004820 halides Chemical class 0.000 abstract description 7
- 239000000243 solution Substances 0.000 description 14
- 238000000034 method Methods 0.000 description 10
- 239000012266 salt solution Substances 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 150000002367 halogens Chemical class 0.000 description 3
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 235000009852 Cucurbita pepo Nutrition 0.000 description 1
- 241000219104 Cucurbitaceae Species 0.000 description 1
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical class [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000012295 chemical reaction liquid Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000000635 electron micrograph Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03C—PHOTOSENSITIVE MATERIALS FOR PHOTOGRAPHIC PURPOSES; PHOTOGRAPHIC PROCESSES, e.g. CINE, X-RAY, COLOUR, STEREO-PHOTOGRAPHIC PROCESSES; AUXILIARY PROCESSES IN PHOTOGRAPHY
- G03C1/00—Photosensitive materials
- G03C1/005—Silver halide emulsions; Preparation thereof; Physical treatment thereof; Incorporation of additives therein
- G03C1/015—Apparatus or processes for the preparation of emulsions
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F27/00—Mixers with rotary stirring devices in fixed receptacles; Kneaders
- B01F27/80—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis
- B01F27/91—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis with propellers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F27/00—Mixers with rotary stirring devices in fixed receptacles; Kneaders
- B01F27/05—Stirrers
- B01F27/11—Stirrers characterised by the configuration of the stirrers
- B01F27/15—Stirrers with tubes for guiding the material
-
- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03C—PHOTOSENSITIVE MATERIALS FOR PHOTOGRAPHIC PURPOSES; PHOTOGRAPHIC PROCESSES, e.g. CINE, X-RAY, COLOUR, STEREO-PHOTOGRAPHIC PROCESSES; AUXILIARY PROCESSES IN PHOTOGRAPHY
- G03C2200/00—Details
- G03C2200/09—Apparatus
Abstract
Description
【発明の詳細な説明】
（Ａ）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 (A) Industrial Field of Application The present invention relates to an apparatus for producing silver halide photographic emulsions, and more specifically to a method for producing halogen emulsions with a narrow grain size distribution and uniform grain crystal habit even in the case of mass production. The present invention relates to a silver halide photographic emulsion production apparatus capable of producing silver halide grains.
ＣＢ）従来技術及びその問題点
粒径分布の狭い均一晶癖のハ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
，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。CB) Prior art and its problems U.S. Pat.
British Patent No. 1,323,464, US Patent No. 3
, 692,283, Japanese Patent Publication No. 55-10545, etc. are known.
これらの装置は、水溶性錫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、粒子晶癖の均一なハ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 tin salts and water-soluble halogen salts, and to simplify the manufacturing process of silver halide photographic emulsions. The shape of the halogen salt solution and the supply method of the halogen salt aqueous solution and silver salt aqueous solution have been improved. However, with these techniques, it is difficult to produce silver halide grains with a 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.
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、撹拌翼による吐出流
を液流肌刷板によって鉛直流上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
は未だ充分ではなく、粒径分布の充分に狭い／％ロゲン
化銀粒子を製造すること力（できなかった。On the other hand, Japanese Patent Application Laid-Open No. 57-92524 discloses that the uniformity of the circulation flow of the liquid throughout the reaction vessel was improved by converting the discharge flow from the stirring blade into a vertical flow using a liquid flow plate. An apparatus for producing a silver halide emulsion is disclosed. However, even with this technique, the circulation of the liquid is still insufficient, and it has not been possible to produce silver halide grains with a sufficiently narrow particle size distribution/%.
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６０−
１１７８３４号公報に開示した。The present inventors improved the prior art and developed a silver halide photographic emulsion production apparatus capable of producing silver halide grains with a narrow grain size distribution and uniform grain crystal habit.
It was disclosed in Publication No. 117834.
かかる技術にもとすくハロゲン化銀写真乳剤の製造装置
を第１図、第４図、および第５図に示す。An apparatus for producing a silver halide photographic emulsion that is suitable for this technique is shown in FIGS. 1, 4, and 5.
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口部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シ各々稀釈し、前記混合器２に設け
られた撹拌翼４によって両反応液を急激に攪拌混合して
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よシ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 an opening 21 at its lower end.
A halogen salt aqueous solution and a silver salt aqueous solution are supplied from pipes 3 and 3'.
The two reaction solutions are diluted with the aqueous protective colloid solution in the mixer 2, and the two 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 circulation in the reaction vessel mixer and uniformizing the growth process of individual silver halide grains, thereby improving the grain size distribution. This method produces narrow silver halide grains.
本発明者等はかかる技術にもとすき、よ）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シ粒径分布の狭いハロゲン
化銀粒子は混合器内撹拌翼回転数をたかめ、混合器導通
路よシ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。The present inventors are interested in such technology, and have continued to conduct intensive studies on production equipment for silver halide grains with a narrow particle size distribution and production equipment suitable for production of large amounts of silver halide grains, and have found that such 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 discharge rate from the mixer conduit.
しかしながら効率的に多量のノーロゲン化銀粒子を製造
するためにはハロゲン塩水溶液と銀塩水溶液の濃度及び
供給速度を増大しなければならず、その場合、高濃度の
ハロゲン塩水溶液と銀塩水溶液が反応し異形粒子が生成
するという問題がある。However, in order to efficiently produce a large amount of silver nohalide grains, it is necessary to increase the concentration and supply rate of the halide aqueous solution and silver salt aqueous solution. There is a problem in that the reaction generates irregularly shaped particles.
（Ｃ）発明の目的
本発明の目的は前記第１図、第４図及び第５図に示され
る従来技術を改良しよシ粒径分布が狭く、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を提供することにある。本発明
の他の目的はハロゲン化銀粒子を効率的に多量製造する
ことを可能ならしめるハロゲン化銀写真乳剤の製造装置
を提供することにある。(C) Purpose of the Invention The purpose of the present invention is to improve the prior art shown in FIGS. 1, 4 and 5. Silver halide grains having a narrow grain size distribution and uniform grain crystal habit can be produced. An object of the present invention is to provide an apparatus for producing a silver halide photographic emulsion. Another object of the present invention is to provide an apparatus for producing a silver halide photographic emulsion, which makes it possible to efficiently produce large quantities of silver halide grains.
ＣＤ）発明の構成
本発明の目的は、反応容器中に撹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、銀塩水溶液及び保護コロイ
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撹拌翼
回転軸方向の鉛直流となるように充分な役拌翼回転軸方
向長さをもち、撹拌翼回転軸方向に開口する仮数の導通
路よフなるハロゲン化銀写真乳剤の製造装置において、
該下端部開口部を２個以上有し、ハロゲン塩水溶液と銀
塩水溶液を別々の該開口部から導入するようにしたハロ
ゲン化銀写真乳剤の製造装置によって達成された。CD) Structure of the Invention The 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 halogen salt aqueous solution, a silver salt aqueous solution and a protective colloid aqueous solution in the lower end thereof. 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 flow to pass through the stirring blade. In an apparatus for producing a silver halide photographic emulsion, the length of the stirring blade is sufficient in the direction of the rotational axis so that a vertical flow occurs in the direction of the rotational axis, and the mantissa conductive path is opened in the direction of the rotational axis of the stirring blade.
This was achieved by a silver halide photographic emulsion producing apparatus having two or more openings at the lower end, and having an aqueous halide solution and an aqueous silver salt solution introduced through separate openings.
以下添付図面にもとすき本発明の実施態様について説明
する。第１図は本発明を適用することのできるハロゲン
化銀写真乳剤製造装置の概略断面図であシ、第２図及び
第３図は本発明に用いられる混合器２の拡大縦断面図で
ある。Embodiments of the present invention will be described below with reference to the accompanying drawings. FIG. 1 is a schematic sectional view of a silver halide photographic emulsion manufacturing apparatus to which the present invention can be applied, and FIGS. 2 and 3 are enlarged longitudinal sectional views of a mixer 2 used in the present invention. .
ハロゲン塩水溶液と銀塩水溶液はそれぞれ供給管３．３
”ｅ通して反応容器１内に設けられた混合器２の下端部
開口部２１．２１′へ別々に連続的に供給される。反応
容器１には保護コロイド水溶液が満たされておシ、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。Supply pipe 3.3 for halogen salt aqueous solution and silver salt aqueous solution, respectively.
The reaction vessel 1 is filled with a protective colloid aqueous solution, and the mixture is mixed. The container 2 is provided below the surface of the aqueous protective colloid solution, and the inside of the mixer 2 is filled with the aqueous protective colloid solution.
反応容器１中の保護コロイド水溶液は該混合器２の作用
によシ、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。Due to the action of the mixer 2, the aqueous protective colloid solution in the reaction vessel 1 is always caused to convect across 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に円形又は円筒形の
開口部２１．２１′ヲ有しておシ、前記円筒形ケーシン
グ上端部に撹拌翼回転軸５の方向にのみ開口する横断面
円形の導通路６を有している。The mixer 2 has a circular or cylindrical opening 21, 21' at the lower end of the cylindrical casing, and a circular or cylindrical opening 21, 21' at the upper end of the cylindrical casing, which has a circular cross section and opens only in the direction of the stirring blade rotating shaft 5. It has a conduction path 6.
導通路６は吐出流を鉛直流にするための充分な撹拌翼回
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
対する導通路長さ値の比として０．０１以上の範囲にあ
るのが好ましい。混合器２には鉛直方向の回転軸５に取
付けられたピッチドパドル型撹拌翼４が設けられている
。撹拌翼４は、供給管３．３′を通して円筒形ケーシン
グ下端部開口部２１．２１’に別々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フ稀釈された
のち、この両反応液を急激に攪拌混合して反応せしめハ
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へ排出せしめるものであ
る。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 mixer 2 is provided with pitched paddle type stirring blades 4 attached to a vertical rotating shaft 5. The stirring blades 4 are used to feed both reaction solutions, which are separately supplied to the lower end opening 21.21' of the cylindrical casing through the supply pipe 3.3', after they have been diluted with the protective colloid aqueous solution in the mixer 2. Both reaction solutions are stirred and mixed rapidly to react and produce silver halide particles, and the produced silver halide particles are immediately discharged from the conduit 6 to the outside of the mixer 2 and above into the protective colloid aqueous solution in the reaction vessel 1. It is something.
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２図及び第３図に示す構成のものに限定さ
れることなく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 silver halide photographic emulsion manufacturing apparatus used in the present invention is not limited to the configuration shown in FIGS. Needless to say, changes are possible.
本発明は、混合器内に供給されたハロゲン塩水溶液と銀
塩水溶液の反応によって生成したハロゲン化銀粒子ｅｆ
ｆｌ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、再び混合器ヘリサイクルさせる。The present invention provides silver halide particles ef produced by a reaction between a halide aqueous solution and a silver salt aqueous solution supplied in a mixer.
After being discharged to the outside of the mixer along with the discharge flow of fl stirring blades, it is circulated within the reaction vessel and recycled to the mixer again.
このリサイクル運動の繰返しの中でハロゲン化銀粒子を
生長させる過程において、高濃度のハロゲン塩水溶液と
銀塩水溶液の反応によって異形粒子が生成するのを防止
し、粒径分布が狭く、粒子晶癖の均−外ハロゲン化銀粒
子の製造を、ハロゲン塩水溶液と銀塩水溶液を混合器内
に別々に導入する開口部を２個以上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 process of growing silver halide grains through the repetition of this recycling movement, the reaction between a highly concentrated halogen salt aqueous solution and a silver salt aqueous solution prevents the formation of irregularly shaped grains, resulting in a narrow grain size distribution and grain crystal habit. The production of uniform silver halide grains was realized using a silver halide photographic emulsion production apparatus having two or more openings for separately introducing an aqueous halide solution and an aqueous silver salt solution into a mixer.
本発明はいわゆるシングルジェット法、ダブルジェット
法、コントロールダブルジェット法等各種のハロゲン化
銀乳剤の製造方法に対し広汎に適用しうるが、特にコン
トロールダブ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、ハロゲン塩水溶液と銀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（懸濁したハロゲン
化銀粒子を含む保護コロイド水溶液）中の銀イオン濃度
を比較的容易に、予め設定した値に維持することが可能
であシ、ハロゲン化銀写真乳剤製造上極めて大きな利点
を有している。The present invention can be widely applied to various silver halide emulsion manufacturing methods such as the so-called single jet method, double jet method, and controlled double jet method. Since the reaction can be carried out quickly and completely, the added amounts of the halide salt aqueous solution and the silver salt aqueous solution are maintained in approximately equal amounts in the dispersion (protective colloid aqueous solution containing suspended silver halide particles). It is possible to maintain the silver ion concentration at a predetermined value relatively easily, which has an extremely large advantage in producing silver halide photographic emulsions.
（Ｅ）実施例 以下本発明の効果を具体的な実施例により例証する。(E) Examples The effects of the present invention will be illustrated below using specific examples.
次の３穏類の溶液を調製した。The following trimodal solutions were prepared.
（水を加えて１５，０ＯＯＣＨに仕上げる。(Add water to make 15.0OOCH.
製造装置としては第１図、第２図に示す構成のものを用
いた。すなわち、溶液〔Ａ）を半球底円筒形反応容器（
直径４００ｍ）に満たし、溶液〔Ｂ〕および［：Ｃ：］
を管３．３′及び下端部開口部２１．２１′を通して反
応温度６０℃で添加時間３０分間及び６０分間の場合に
ついて定速（３０分間の場合３３４ ｃｒｙ／ｍｉｎ
、 ６０分間の場合１６７シｍ１ｎ）で連続的に添加し
た。The manufacturing apparatus used was one having the configuration shown in FIGS. 1 and 2. That is, the solution [A] was placed in a cylindrical reaction vessel with a hemispherical bottom (
400 m in diameter) and solution [B] and [:C:]
through tube 3.3' and lower end opening 21.21' at a reaction temperature of 60° C. at a constant rate for addition times of 30 and 60 minutes (334 cry/min for 30 minutes).
, 167 m1n for 60 minutes) was added continuously.
混合器はケーシングが直径８０■、高さ７０ｔｔｔｓの
円筒形で下端部２１．２１′は直径２５日で開口してお
り、上端部導通路６は直径２５ｍで鉛直方向に２０瓢の
長さである。撹拌翼４は翼長２０ｍ＋の角度４５°ピツ
チドパドルを用い回転数２００Ｏｒｐｍで回転させた。The mixer has a cylindrical casing with a diameter of 80 cm and a height of 70 ttts, and the lower end 21.21' is open with a diameter of 25 days, and the upper end conduit 6 has a diameter of 25 m and a length of 20 gourds in the vertical direction. be. The stirring blade 4 was a pitched paddle having a blade length of 20 m+ and an angle of 45°, and was rotated at a rotational speed of 200 rpm.
一方、上記本発明の実施例において、第４図の如く、下
端部２１が直径３０日で開口している混合器（他の構成
は上記本発明例と同じ）を用い、上記実施例と同じ条件
で比較実験を行った。On the other hand, in the embodiment of the present invention described above, as shown in FIG. A comparative experiment was conducted under the following conditions.
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υ平均粒径、標準偏差及び異形粒子個数につい
て測定した。その結果は表−１の通シであった。The silver halide grains thus obtained were measured for υ average grain size, standard deviation, and number of irregularly shaped grains using electron micrographs. The results were as shown in Table 1.
表−１
比較実験におけるハロゲン化銀粒子の大部分は（１，Ｏ
，Ｏ）面を有する結晶であったが、異形粒子ははまぐり
呈結晶であった。又添加時間が短い場合、反応液供給速
度が犬きくなシ、比較実験では、明らかに異形粒子が増
加するのに対し、本発明のハロゲン化銀写真乳剤製造装
置を用いた場合、反応液供給速度に関係なく異形粒子の
生成は皆無であった。Table 1 Most of the silver halide grains in comparative experiments were (1,O
, O) planes, but the irregularly shaped particles were clam crystals. In addition, when the addition time is short, the reaction solution supply rate is too slow, and in comparative experiments, the number of irregularly shaped grains clearly increases. No irregularly shaped particles were produced regardless of the speed.
ＣＦ）発明の効果
以上の記載から明らかなように、本発明によシ次のよう
な効果が得られる。CF) Effects of the Invention As is clear from the above description, the following effects can be obtained by the present invention.
（１）本発明のハロゲン化銀写真乳剤製造装置を用い、
ハロゲン塩水溶液と銀塩水溶液を別々の混合器ケーシン
グ下端部開口部から導入することによって、効率的に多
量に且つ粒径分布が狭く、均一晶癖のハロゲン化銀写真
乳剤が製造できる。(1) Using the silver halide photographic emulsion manufacturing apparatus of the present invention,
By introducing an aqueous halogen salt solution and an aqueous silver salt solution through separate openings at the lower end of the mixer casing, a silver halide photographic emulsion with a uniform crystal habit and a narrow particle size distribution can be efficiently produced in large quantities.
（２）粒径分布の狭い、均一晶癖のハロゲン化銀が製造
できるので写真性能の向上、とくに省銀址化が可能にな
る。(2) Since silver halide with a narrow grain size distribution and uniform crystal habit can be produced, photographic performance can be improved, and in particular, silver waste can be saved.
第１図は従来の技術にもとすく、及び本発明を適用する
ことのできる装置の概略縦断図、第２図、第３図は本発
明による装置の混合器部分の拡大縦断面図、第４図は従
来技術にもとすく混合器部分の拡大縦断面図、第５図は
第４図の平面図である。
図中、１は反応容器、２は混合器、３．３’は反応液供
給管、４は撹拌翼、５は撹拌翼回転軸、６は導通路、２
１．２１’は下端部開口部第１ｚ
第２図 第３図
第４図
第５図FIG. 1 is a schematic longitudinal sectional view of a device which is similar to the prior art and to which the present invention can be applied; FIGS. 2 and 3 are enlarged longitudinal sectional views of a mixer portion of the device according to the present invention; FIG. 4 is an enlarged vertical sectional view of a mixer portion according to the prior art, and FIG. 5 is a plan view of FIG. 4. In the figure, 1 is a reaction container, 2 is a mixer, 3.3' is a reaction liquid supply pipe, 4 is a stirring blade, 5 is a stirring blade rotating shaft, 6 is a conductive path, 2
1.21' is the lower end opening 1z Figure 2 Figure 3 Figure 4 Figure 5
Claims (1)
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、銀塩水溶液及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撹拌翼回転軸方向の鉛
直流となるように充分な撹拌翼回転軸方向長さをもち、
撹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、該下端部開口部
を２個以上有し、ハロゲン塩水溶液と銀塩水溶液を別々
の該開口部から導入するようにしたことを特徴とするハ
ロゲン化銀写真乳剤の製造装置。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 an opening at the lower end for introducing a halogen salt aqueous solution, a silver salt aqueous solution, and a protective colloid aqueous solution into the mixer. and has an opening at the upper end for discharging the silver halide particles generated in the mixer, and the upper end opening is arranged so that the discharged liquid flow becomes a vertical flow in the direction of the rotation axis of the stirring blade. The stirring blade has sufficient length in the rotation axis direction,
A silver halide photographic emulsion manufacturing apparatus comprising a plurality of conductive passages opening in the rotational axis direction of the stirring blade, which has two or more lower end openings, and a halogen salt aqueous solution and a silver salt aqueous solution are supplied from separate openings. 1. An apparatus for producing a silver halide photographic emulsion, characterized in that:
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61236721A JPS6389837A (en) | 1986-10-03 | 1986-10-03 | Apparatus for producing photographic silver halide emulsion |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61236721A JPS6389837A (en) | 1986-10-03 | 1986-10-03 | Apparatus for producing photographic silver halide emulsion |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS6389837A true JPS6389837A (en) | 1988-04-20 |
Family
ID=17004794
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP61236721A Pending JPS6389837A (en) | 1986-10-03 | 1986-10-03 | Apparatus for producing photographic silver halide emulsion |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS6389837A (en) |
-
1986
- 1986-10-03 JP JP61236721A patent/JPS6389837A/en active Pending
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