JPS61103148A - Device for preparing silver halide emulsion - Google Patents
Device for preparing silver halide emulsionInfo
- Publication number
- JPS61103148A JPS61103148A JP22546284A JP22546284A JPS61103148A JP S61103148 A JPS61103148 A JP S61103148A JP 22546284 A JP22546284 A JP 22546284A JP 22546284 A JP22546284 A JP 22546284A JP S61103148 A JPS61103148 A JP S61103148A
- Authority
- JP
- Japan
- Prior art keywords
- emulsion
- silver halide
- pot
- halide emulsion
- zirconium
- 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
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
-
- 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】
［産業上の利用分野］
本発明はハロゲン化銀乳剤の製造装置に関し、詳しくは
ハロゲン化銀乳剤の写真特性に悪影響を与えず耐久性も
良好な材質を用いたハロゲン化銀乳剤の製造装置に関す
る。Detailed Description of the Invention [Field of Industrial Application] The present invention relates to an apparatus for producing a silver halide emulsion, and more specifically, the present invention relates to an apparatus for producing a silver halide emulsion. The present invention relates to an apparatus for producing a silver oxide emulsion.
［従来技術］
写真用ハロゲン化銀乳剤は、ハロゲン塩溶液と硝酸銀溶
液とゼラチンの存在下に混合することにより作られる。[Prior Art] Photographic silver halide emulsions are made by mixing a halide salt solution, a silver nitrate solution, and gelatin in the presence of gelatin.
上記溶液の混合の結果生じるハロゲン化銀は、混合する
ハロゲン塩の種類、濃度、硝ｌ銀溶液の］Ｌアンモニア
の有無や添加量、混合方法、混合速度、その他共存する
物質、反応温度、時間係数等に大きく影響を受け、Ｒ柊
的に写実特性に影響を与えることになる。The silver halide produced as a result of mixing the above solutions is determined by the type and concentration of the halide salt to be mixed, the presence or absence of L ammonia in the silver nitrate solution, the amount added, the mixing method, the mixing speed, other coexisting substances, reaction temperature, time. It is greatly influenced by coefficients, etc., and has a large effect on the realism characteristics.
近年、特に単分散乳剤と言われる粒径分布の極めて狭い
乳剤の製造が行なわれており、匙剤の製造工程における
条件の厳密さがより一層要求されている。In recent years, emulsions with extremely narrow particle size distributions, particularly so-called monodisperse emulsions, have been produced, and stricter conditions are required in the process of producing spoons.
従来、このハロゲン化銀乳剤の製造に用いられる装置の
材質としては、その耐久性、価格、入手の容易さ等から
５ＬＪＳ３０４．５ＬＪＳ３０６等のステンレス鋼が一
般に用いられている。Conventionally, stainless steel such as 5LJS304.5LJS306 has been generally used as the material for the equipment used to produce this silver halide emulsion due to its durability, price, ease of availability, etc.
ところで、前記単分散乳剤は重金属イオンの影響を受け
やすく、例えば、ニッケルＮ１、コバルトＣＯ１鉄「ｅ
１モリブデンＭｏ、クロムＱｒ等の重金属のイオンはｐ
ｐｍ〜Ｉ）ｌ）ｂオーダーの液中含有用で乳剤性能に影
響を与える。By the way, the monodispersed emulsion is easily affected by heavy metal ions, such as nickel N1, cobalt CO1 iron "e".
1 Ions of heavy metals such as molybdenum Mo and chromium Qr are p
It is included in the liquid on the order of pm to I)l)b and affects emulsion performance.
従って、Ｃ「およびＮ１を含む５ＬＩＳ３０４系等のス
テンレス鋼の利用は好ましいものとは言えなかった。Therefore, the use of stainless steels such as the 5LIS304 series containing C" and N1 could not be said to be preferable.
その様な事情から、装置の接液部にグラスライニング、
テフロンゴム１−、シリコン、テフロンゴム等を用いる
ことも行なわれているが、これらの利用も次に挙げる理
由により問題があった。Due to such circumstances, glass lining,
Although Teflon rubber 1-, silicone, Teflon rubber, etc. have been used, there are also problems with the use of these materials for the following reasons.
１）Ｍ久性に劣る。２）コスト的に高い、３）加工性が
悪い。４）系の温度制御が困難、、５）添加剤の影響が
ある。６）制御用部材として不適である。1) Poor M durability. 2) High cost; 3) Poor workability. 4) It is difficult to control the temperature of the system, 5) There is an influence of additives. 6) Not suitable as a control member.
さらに、近年開発の著しいセラミックス材の利用も考え
られるが、加工性、！ｉＦ８等の点において問題がある
。Furthermore, the use of ceramic materials, which have been significantly developed in recent years, can be considered, but the processability! There is a problem with iF8 etc.
以上述べた如く、ハロゲン化銀乳剤の製造装置の材質は
、写貴乳剤の特性に悪影響を与えず、安定な生産を保障
するものの開発が望まれていた。As mentioned above, it has been desired to develop a material for silver halide emulsion manufacturing equipment that does not adversely affect the properties of the emulsion and ensures stable production.
［発明の目的］
本発明は上記の問題点に鑑み為されたものであり、本発
明の目的は、写真乳剤特性に悪影響を与えず、安定な生
産を保障するハロゲン化銀乳剤の製造装置を提供するこ
とである。[Object of the Invention] The present invention has been made in view of the above-mentioned problems, and an object of the present invention is to provide a silver halide emulsion manufacturing apparatus that does not adversely affect photographic emulsion properties and ensures stable production. It is to provide.
［発明の構成］
本発明者等は鋭意検討の結果、本発明の上記目的は、少
なくとも反応液供給釜、ハロゲン化銀晶析装置、各部を
連結するバイブラインおよび流Ｍ制御弁を有するハロゲ
ン化銀乳剤の製造装置において、接液部が金属ジルコニ
ウムまたはジルコニウム合金である部分を有するハロゲ
ン化銀乳剤の製造装置により達成されることを見い出し
た。[Structure of the Invention] As a result of intensive studies, the present inventors have found that the above-mentioned object of the present invention is to provide a halogenation system having at least a reaction liquid supply pot, a silver halide crystallizer, a vibrate line connecting each part, and a flow M control valve. It has been found that the present invention can be achieved by a silver halide emulsion manufacturing apparatus in which the liquid contact part has a portion made of metal zirconium or a zirconium alloy.
【発明の具体的構成］
本発明は、ハロゲン化銀乳剤の製造装置の接液部の少な
くとも一部に金属ジルコニウムまたはジルコニウム合金
を用いることに特徴があるが、ジルコニウムは、例えば
、日本写真学会誌、７゜１５ （１９４１）の記載によ
れば、乳剤混合時のジルコニウムの存在は感光度および
カブリを低下すると報告されているにもかかわらず、金
属ジルコニウムまたはジルコニウム合金を乳剤製造装置
に用いて良好な結果を得たものである。Specific Structure of the Invention The present invention is characterized in that metallic zirconium or a zirconium alloy is used for at least a part of the liquid contact part of a silver halide emulsion manufacturing apparatus. , 7゜15 (1941), although it has been reported that the presence of zirconium during emulsion mixing reduces photosensitivity and fog, metallic zirconium or zirconium alloys have not been successfully used in emulsion manufacturing equipment. The results obtained were as follows.
本発明の乳剤製造装置は、少なくとも１部に金属ジルコ
ニウムまたはジルコニウム合金を用いるが、ジルコニウ
ム合金としては、例えば、ＡＱ−２ｒ 、ＡＬＩ −１
ｒ 、Ｃｕ −ｚｒ 、ｃｒ−ｚｒ、Ｆｅ −Ｚｒ 、
Ｎｉ −７ｒ 、 Ｍｏ −Ｚｒ 、 Ｐｔ −２ｒ
、 Ｓｉ −Ｚｒ 、 Ｔａ −Ｚｒ ％Ｔｉ −Ｚ
ｒ １）−Ｉｆ−ＺｒおよびＮｂ −Ｚｒ ’Ｊが挙げ
られ、これらの一種または２種以上を組み合わせて用い
ることができる。The emulsion manufacturing apparatus of the present invention uses metallic zirconium or a zirconium alloy for at least a portion thereof, and examples of the zirconium alloy include AQ-2r, ALI-1
r, Cu-zr, cr-zr, Fe-Zr,
Ni-7r, Mo-Zr, Pt-2r
, Si-Zr, Ta-Zr%Ti-Z
r1)-If-Zr and Nb-Zr'J, which can be used alone or in combination of two or more.
その合金におけるジルコニウム含有率としては、モル比
で２０％以上が好ましい。The zirconium content in the alloy is preferably 20% or more in terms of molar ratio.
以下、本発明を図面により具体的に説明する。Hereinafter, the present invention will be specifically explained with reference to the drawings.
図面は本発明の一実施例を示し、第１図は本発明のハロ
ゲン化銀乳剤の製造装置の説明図である。The drawings show an embodiment of the present invention, and FIG. 1 is an explanatory diagram of an apparatus for producing a silver halide emulsion of the present invention.
図中１ｏは、硝酸銀水溶液ｖＡ製糸における銀溶解釜で
あり、１１は、銀溶解釜１０に設けられる撹拌翼である
。１２は、バイブラインで、１３は再結晶皿である。硝
酸銀は再結晶により精製した後、所定濃度に再溶解して
ＦＩ４駿銀水溶液供給釜２０に送られる。２１は該硝酸
銀水溶液供給釜２０に設けらる撹拌スであり、２２は、
供給釜２０とハロゲン化銀乳剤調製釜４０（晶析装置）
とを結ぶバイブラインである。同バイブライン２２には
途中にポンプ２３と流量計２４と制御弁２５が設けられ
ており、ポンプ２３、制御弁２５は乳剤調製釜４０中に
設けられたＩ）Ａｇセンサー（図示せず）、ｐ ｌ−Ｉ
センサー（図示せず）等からの信号により、その硝酸銀
水溶液の供給量をコントロールする如くなっている。一
方ハロゲン塩水溶液は、所定の濃度に保持されてハロゲ
ン塩水溶液供給釜３０から、該ハロゲン塩水溶液供給釜
３０と乳剤調製釜４０を結ぶバイブライン３２を経て乳
剤調製釜４０に供給される。また、同バイブライン３２
には途中にポンプ３３と流量計３４と制御弁３５が設け
られており、ポンプ３３、制御弁３５は乳剤調製釜４０
中に設けられたｐＡ９Ａｇセンサー示せず）、１１セン
サー（図示せず）等からの信号により、そのハロゲン塩
水溶液の供給量をコントロールする如くなっている。ま
た、各部にはそれぞれの撹拌ｒＩ４２１．３１．４１が
設けられている。In the figure, 1o is a silver dissolving pot in the silver nitrate aqueous solution vA yarn spinning, and 11 is a stirring blade provided in the silver dissolving pot 10. 12 is a vibrine, and 13 is a recrystallization dish. After the silver nitrate is purified by recrystallization, it is redissolved to a predetermined concentration and sent to the FI4 silver aqueous solution supply tank 20. 21 is a stirrer provided in the silver nitrate aqueous solution supply tank 20, and 22 is
Supply pot 20 and silver halide emulsion preparation pot 40 (crystallizer)
It is a vibe line that connects them. The vibration line 22 is provided with a pump 23, a flow meter 24, and a control valve 25 in the middle, and the pump 23 and the control valve 25 are connected to an I) Ag sensor (not shown) provided in the emulsion preparation pot 40; p l-I
The supply amount of the silver nitrate aqueous solution is controlled by a signal from a sensor (not shown) or the like. On the other hand, the halogen salt aqueous solution is maintained at a predetermined concentration and is supplied from the halogen salt aqueous solution supply vessel 30 to the emulsion preparation vessel 40 via a vibrating line 32 connecting the halogen salt aqueous solution supply vessel 30 and the emulsion preparation vessel 40 . In addition, the same vibe line 32
A pump 33, a flow meter 34, and a control valve 35 are provided in the middle of the emulsion preparation tank 40.
The supply amount of the halogen salt aqueous solution is controlled by signals from the pA9Ag sensor (not shown), 11 sensor (not shown), etc. provided therein. Each part is also provided with its own stirring rI421.31.41.
上記各部材の少なくとも接液部が金属ジルコニウムまた
はジルコニウム合、金である部分を有するように構成す
る。これは、各部材全体を金属ジルコニウムまたはジル
コニウム合金で形成することはもちろＩν、反応液と接
触する内壁面の金属ジルコニウムまたはジルコニウム合
金でライニング処理する等のように部材の一部に使用す
ることも包含される。なお、ジルコニウム以外の材質で
形成する部分でも、接液部には５Ｕ８３０４等のスレン
レス鋼を用いないのが好ましい。At least the liquid contact portion of each of the above members is configured to have a portion made of metal zirconium, a zirconium alloy, or gold. This can be used not only for the entire member to be made of metallic zirconium or zirconium alloy, but also for a part of the member, such as by lining the inner wall surface that comes into contact with the reaction liquid with metallic zirconium or zirconium alloy. is also included. Note that even in parts formed of materials other than zirconium, it is preferable not to use stainless steel such as 5U8304 for liquid contact parts.
また、乳剤ｉｌ製時に重要なものとして、乳剤調製釜４
ｏへの硝酸銀水溶液およびハロゲン塩水溶液等の供給量
をコントロールする制御弁２５．３５があるが、これら
は、上記各溶液の供給量を正確にコントロールできるも
のであればどれでも用いることができ、例えば、ニード
ル弁等が好ましく用いられる。その場合においては、特
にその加工性、硬度、耐久性、耐薬品性等の点において
当業界で従来用いられていた弁部材よりも金属ジ’′ｊ
１ ルコニウムおよびジルコニウム合金が優れ
ているものである。また、ニードル弁の様々複雑な構造
物において、金属ジルコニウムまたはジルコニウム合金
を用いることが、とくに有効である。In addition, the emulsion preparation pot 4 is important when producing emulsion IL.
There is a control valve 25.35 that controls the supply amount of the silver nitrate aqueous solution and the halogen salt aqueous solution etc. to the o, but any valve can be used as long as it can accurately control the supply amount of each of the above solutions For example, a needle valve or the like is preferably used. In that case, metal parts are better than valve members conventionally used in this industry, especially in terms of workability, hardness, durability, chemical resistance, etc.
1. Ruconium and zirconium alloys are superior. It is also particularly advantageous to use metallic zirconium or zirconium alloys in various complex structures of needle valves.
本発明の製造装置は、ハロゲン化銀乳剤の製造方法にお
けるアンモニア法、中性法、醒性法のいずれにも好まし
く適用できる。また、当業界で用いられるシングルジェ
ット混合法、ダブルジェット混合法、コンドロールドダ
ブルジェット混合法のいずれにも好ましく適用でき、特
にコンドロールドダブルジェット混合法の関数添加制御
仕込に適用してその効果を発揮する。The production apparatus of the present invention can be preferably applied to any of the ammonia method, neutral method, and aqueous method in the production method of silver halide emulsions. In addition, it can be preferably applied to any of the single jet mixing method, double jet mixing method, and Chondrold double jet mixing method used in the industry, and is particularly applicable to the function addition control preparation of the Chondrold double jet mixing method. be effective.
さらに、本発明の製造装置は、硝酸銀水溶液の濃度、９
１−１、ハロゲン塩の種類、その水溶液の濃度、１）Ｉ
−１、また使用温度等、当業界で用いられる範囲のいず
れにおいても好ましく適用できる。Furthermore, the production apparatus of the present invention has a concentration of silver nitrate aqueous solution of 9.
1-1. Type of halogen salt, concentration of its aqueous solution, 1) I
-1, and the operating temperature can be preferably applied within any range used in the art.
以上述べた如く、本発明のハロゲン化銀乳剤の製造装置
では、接液部が金属ジルコニウムまたはジルコニウム合
金である部分を有するものであれば、本発明の効果を得
られるが、好ましくは、少なくとも流量制御弁が金属ジ
ルコニウムまたはジルコニウム合金からなるのであり、
より好ましくは、接液部が実質的にスレンレ鋼でない部
材からなるものであり、さらに好ましくは、前記金属ジ
ルコニウムまたはジルコニウム合金からなる流ｆｆｉ
ｆｉｌＪ ｔ［ｌ弁がニードル弁であるものである。As described above, in the silver halide emulsion manufacturing apparatus of the present invention, the effects of the present invention can be obtained as long as the wetted part has a portion made of metallic zirconium or a zirconium alloy. The control valve is made of metallic zirconium or zirconium alloy,
More preferably, the liquid contact part is made of a member that is not substantially made of stainless steel, and even more preferably, the liquid contact part is made of a member that is not substantially made of stainless steel, and even more preferably, the liquid contact part is made of a member that is not substantially made of stainless steel.
The filJ t[l valve is a needle valve.
［発明の具体的効果］
以上説明した如く、本発明によれば接液部が金属ジルコ
ニウムまたはジルコニウム合金である部分を有する製造
装置により、写奥乳剤特性に悪影響を与えず１．装置の
耐久性が向上することによりハロゲン化銀乳剤の安定な
生産を保障することができる。[Specific Effects of the Invention] As explained above, according to the present invention, the manufacturing apparatus having the liquid contact part made of metallic zirconium or a zirconium alloy can achieve the following effects without adversely affecting the photographic depth emulsion characteristics. By improving the durability of the equipment, stable production of silver halide emulsions can be guaranteed.
［発明の具体的実施例］
以下本発明を実施例によりさらに具体的に説明するが、
本発明の実施の態↑よがこれにより限定されるものでは
ない。[Specific Examples of the Invention] The present invention will be explained in more detail with reference to Examples below.
The embodiments of the present invention are not limited thereto.
ハロゲン化銀乳剤の製造装置を第２図に示す如くに組み
上げた。第２図において第１図と同一番号で示したもの
は第１図と同義であり、説明を省略する。図中２６は酢
酸供給釜、２７は該酢酸供給釜２６と乳剤調製釜４０を
結ぶバイブライン、同バイブライン２７には途中に流量
計２８と制御弁２９が設けられている。３６は第２ハロ
ゲン店供給釜、３７は該第２ハロゲン塩供給釜３６と乳
・剤Ｘ１１１Ｊ ’Ｉ＝ ４０を結ぶバイブライン、
同バイブライン３７には途中に流量計３８とＩＱ御弁３
９が設けられている。５０．５１はそれぞれ流Ｍコント
ロール装置である。An apparatus for producing a silver halide emulsion was assembled as shown in FIG. Components in FIG. 2 denoted by the same numbers as in FIG. 1 have the same meanings as in FIG. 1, and their explanation will be omitted. In the figure, 26 is an acetic acid supply tank, 27 is a vibration line connecting the acetic acid supply tank 26 and the emulsion preparation tank 40, and the vibration line 27 is provided with a flow meter 28 and a control valve 29 in the middle. 36 is a second halogen salt supply pot; 37 is a vibration line connecting the second halogen salt supply pot 36 and emulsion X111J'I=40;
The same vibe line 37 has a flow meter 38 and an IQ control valve 3 on the way.
9 is provided. 50 and 51 are flow M control devices, respectively.
第２図に示した装置において、２５．２９．３５．３９
で示される制御弁にはニードル弁を用い、さらに図中２
０の硝酸銀水溶液供給釜（以下釜２０という）、４０の
乳剤調整釜（晶析装置、以下、釜４０という）および２
５のニードル制御弁２５（以下弁２５という）のそれぞ
れを、各部分のみ交換可能にして下記表−１に記載の材
質とし、それ以外の装置全工程を、４−６７フ化テフロ
ン（ダイキン社製）を２００μｍの厚さでコーティング
した５ＬＪＳ３０４ステンレス圀を用いた装置とした。In the apparatus shown in Fig. 2, 25.29.35.39
A needle valve is used as the control valve shown in 2.
0 silver nitrate aqueous solution supply pot (hereinafter referred to as pot 20), 40 emulsion adjustment pot (crystallizer, hereinafter referred to as pot 40), and 2
Each of the needle control valves 25 (hereinafter referred to as valves 25) of No. 5 is made replaceable and made of the material listed in Table 1 below. The device was made of 5LJS304 stainless steel coated with a thickness of 200 μm.
使用した１６種類の装置を表−２に示す。Table 2 shows the 16 types of equipment used.
以下１丁１［′Ｉ
表−１
次に、以下に記載した５種類の溶液を用いて沃化銀含有
量が２モル％の立方体沃臭化銀乳剤の製造を行った。Table 1 Next, a cubic silver iodobromide emulsion having a silver iodide content of 2 mol % was prepared using the five types of solutions described below.
溶液Ａ（硝酸銀水溶液供給釜２０に投入）溶液Ｂ（ハロ
ゲン塩供給釜３０に投入）溶液Ｃ（酢酸供給Ｍ２６に投
入）
５６％酢酸水溶Ｗｉ ５６０ｍ文
溶液Ｄ（第２ハロゲン塩供給釜３６に投入）４０％臭化
カリウム溶液 １ｏｏｍｌ溶液口（乳剤調
製釜４０に投入）
乳剤調製釜４０中の溶液Ｅを６０℃で撹拌下に、銀イオ
ン検出電極とＤＨＩ！極を浸し、ｐＨを９．０゜１）Ａ
ｇを９，０ＴＰ−調整した。溶液Ｃと溶液りの流速を制
御してこの値を保ちつつ、新しいハロゲン化銀粒子が発
生しない速度で、コンドロールドダブルジェット法によ
り溶液Ａと８を添加した。添加終了までに要した時間は
５４分であった。Solution A (injected into silver nitrate aqueous solution supply vessel 20) Solution B (injected into halogen salt supply vessel 30) Solution C (injected into acetic acid supply M26) 56% acetic acid aqueous solution Wi 560m solution D (injected into second halogen salt supply vessel 36) ) 40% potassium bromide solution 1 ooml solution port (injected into emulsion preparation pot 40) While stirring solution E in emulsion preparation pot 40 at 60°C, add silver ion detection electrode and DHI! Soak the electrode and adjust the pH to 9.0゜1)A
g was adjusted to 9,0 TP. While controlling the flow rates of solution C and the solution to maintain these values, solutions A and 8 were added by the Chondral double jet method at a rate that did not generate new silver halide grains. The time required to complete the addition was 54 minutes.
上記で製造したハロゲン化銀乳剤を沈澱法で脱塩し、チ
オ硫酸ナトリウムを加え化学増感した後、ポリエステル
支持体上に５．０１１１ ／ＩＩ”の銀量となるように
塗布して感光材料試料を得た。The silver halide emulsion produced above was desalted by a precipitation method and chemically sensitized by adding sodium thiosulfate, and then coated on a polyester support to a silver content of 5.0111/II'' to form a photosensitive material. A sample was obtained.
得られた感光材料試料を通常の方法で露光し、ＣＯＸ現
像液［小西六写真工業株式会社ＩＪＩで現像し、感度を
求めた。The obtained light-sensitive material sample was exposed in a conventional manner and developed with a COX developer [IJI, Konishiroku Photo Industries Co., Ltd., to determine the sensitivity.
上記ハロゲン化銀乳剤の！１１製を表−２に示した各構
成の乳剤製造装置を用いて行ない、以下感光材料の作製
、感度測定までを同様に行なった。Of the above silver halide emulsion! No. 11 was prepared using an emulsion manufacturing apparatus having each configuration shown in Table 2, and the subsequent steps up to the preparation of the light-sensitive materials and sensitivity measurements were carried out in the same manner.
上記で得られた各試料について乳剤性能を感度で示し、
さらに用いた乳剤製造装置の耐久性を以下の如く評価し
た。For each sample obtained above, the emulsion performance is shown by sensitivity,
Furthermore, the durability of the emulsion manufacturing equipment used was evaluated as follows.
感度は、釜２０、釜４０及び弁２５のそれぞれに５ｔＪ
Ｓ３０４に４−６７）化テフロンを２００μｍの厚さで
コーティングした部材を用いた装置から得られた試料を
１００とした比感度で示した。Sensitivity is 5tJ for each of pot 20, pot 40, and valve 25.
The specific sensitivity is expressed as 100 for a sample obtained from an apparatus using a member coated with 4-67) Teflon on S304 to a thickness of 200 μm.
例えば、表−２において、■の５ＵＳ３Ｃ１４行の釜４
０列に示された試料の比感度の！！９８は以下法に耐久
性は、目視上の腐蝕がなく、乳剤の製造装置機能および
動作に影響がなければ０１いずれか一方が劣化した場合
は×とし、艮Ｗ４間の使用により劣化した場合をΔとし
た。For example, in Table 2, pot 4 in row 5US3C14 of ■
The specific sensitivity of the sample shown in column 0! ! 98 is the following method.Durability is 01 if there is no visible corrosion and does not affect the function and operation of the emulsion manufacturing equipment.If either one of them has deteriorated, it is marked as ×, and if it has deteriorated due to use between W4. It was set as Δ.
以と１６の＠置でそれぞれ２回行った平均の結果を表−
２に併せて示す。The table below shows the average results obtained twice at each of the following and 16 @ positions.
It is also shown in 2.
以下全白
表−２の結果から明らかなように、金属ジルコニウムを
それぞれＭ ２０ 、釜４０、弁２５に用いた本発明の
乳剤製造装置から得られた乳剤の感度および装置自身の
耐久性は、他の部材を使用した場合に比較して優れてい
ることがわかる。As is clear from the results in Table 2 below, the sensitivity of the emulsion obtained from the emulsion manufacturing apparatus of the present invention using metallic zirconium for M20, pot 40, and valve 25 and the durability of the apparatus itself are as follows: It can be seen that this is superior compared to cases where other members are used.
図面は本発明の一実施例を示し、第１図および第２図は
ハロゲン化銀乳剤の製造装置の説明図である。
１０・・・銀溶解釜、 １３・・・再結晶皿、２
０・・・硝ＩＩ銀水溶液供給釜、 ２６・・・＃葭洪＠
釜、３０・・・ハロゲン塩水溶液供給釜、
３６・・・第２ハロゲンＪ！ｉ供給釜、１１．２１．３
１．４１・・・撹拌翼、１２．２２．２７．３２．３７
・・・バイブライン、２３．３３・・・ポンプ、
２４．２８．３４．３８・・・流量計、２５ 、 ２９
、３５ 、３９ ・・・酊り御弁 、４０・・・ハロ
ゲン化銀調製釜（晶析装置）、５０．５１・・・ＦＲ１
！コントロール装買手続ネ市正書 （自発）
昭和６１年０１月２２日The drawings show one embodiment of the present invention, and FIGS. 1 and 2 are explanatory diagrams of a silver halide emulsion manufacturing apparatus. 10... Silver melting pot, 13... Recrystallization dish, 2
0...Nitrogen II silver solution supply pot, 26...#Yoshihong@
Pot, 30... Halogen salt aqueous solution supply pot, 36... Second halogen J! i Supply pot, 11.21.3
1.41... Stirring blade, 12.22.27.32.37
...Vibline, 23.33...Pump, 24.28.34.38...Flowmeter, 25, 29
, 35 , 39 ... Drunk goben , 40 ... Silver halide preparation pot (crystallizer), 50.51 ... FR1
! City official document on control purchase procedures (voluntary) January 22, 1986
Claims (1)
を連結するバイブラインおよび流量制御弁を有するハロ
ゲン化銀乳剤の製造装置において、接液部が金属ジルコ
ニウムまたはジルコニウム合金である部分を有すること
を特徴とするハロゲン化銀乳剤の製造装置。In a silver halide emulsion manufacturing apparatus having at least a reaction liquid supply tank, a silver halide crystallizer, a vibrator connecting each part, and a flow rate control valve, it is preferable that the liquid contact part has a part made of metallic zirconium or a zirconium alloy. Characteristic silver halide emulsion manufacturing equipment.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP22546284A JPS61103148A (en) | 1984-10-26 | 1984-10-26 | Device for preparing silver halide emulsion |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP22546284A JPS61103148A (en) | 1984-10-26 | 1984-10-26 | Device for preparing silver halide emulsion |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS61103148A true JPS61103148A (en) | 1986-05-21 |
Family
ID=16829707
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP22546284A Pending JPS61103148A (en) | 1984-10-26 | 1984-10-26 | Device for preparing silver halide emulsion |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS61103148A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02191943A (en) * | 1988-10-31 | 1990-07-27 | Konica Corp | Silver halide photographic sensitive material having superior antistatic performance |
| US5213772A (en) * | 1988-12-22 | 1993-05-25 | Fuji Photo Film Co., Ltd. | Apparatus for forming silver halide grains |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5792523A (en) * | 1980-11-29 | 1982-06-09 | Konishiroku Photo Ind Co Ltd | Method and apparatus for preparation of silver halide particle |
-
1984
- 1984-10-26 JP JP22546284A patent/JPS61103148A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5792523A (en) * | 1980-11-29 | 1982-06-09 | Konishiroku Photo Ind Co Ltd | Method and apparatus for preparation of silver halide particle |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02191943A (en) * | 1988-10-31 | 1990-07-27 | Konica Corp | Silver halide photographic sensitive material having superior antistatic performance |
| US5213772A (en) * | 1988-12-22 | 1993-05-25 | Fuji Photo Film Co., Ltd. | Apparatus for forming silver halide grains |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| EP0634689B1 (en) | Internally doped silver halide emulsions and processes for their preparation | |
| JPS5836762B2 (en) | Method for producing uniformly sized silver halide emulsion | |
| CA1316036C (en) | Process for preparing a photographic emulsion containing tabular grains having narrow size distribution | |
| US3672900A (en) | Fogged direct-positive emulsion production by increased flow of silver halide-forming precipitants in grain-ripenerfree acidic medium | |
| JPS6133177B2 (en) | ||
| JPS6259053B2 (en) | ||
| JPS61103148A (en) | Device for preparing silver halide emulsion | |
| JPH04318544A (en) | Silver halide emulsion for processing of inclusion of physical development for dissolution | |
| EP0397125B1 (en) | Silver halide emulsions having improved low intensity reciprocity characteristics and processes of preparing them | |
| JPS59212826A (en) | Preparation of silver halide photographic emulsion | |
| JP2000321696A (en) | Preparation of emulsion | |
| Nietz | The theory of development | |
| JPH06235992A (en) | Halogenated silver photograph emulsion containing contrast-improved type particle-surface modifier | |
| JPH0439060B2 (en) | ||
| JPS583532B2 (en) | Method for producing silver halide photographic emulsion | |
| JPH05204069A (en) | Manufacture of photographic emulsion | |
| US3951656A (en) | Direct-positive silver halide emulsion fogged with a cyanoborohydride anion | |
| JPH08248545A (en) | Method for reaction of plurality of components | |
| JPH10333267A (en) | Method for processing silver chloroiodide emulsion | |
| EP0047975B1 (en) | Direct-positive photographic element and method for producing a direct-positive silver halide emulsion | |
| US6033842A (en) | Preparation of silver chloride emulsions having iodide containing grains | |
| JPS59214028A (en) | Preparation of silver halide photographic emulsion | |
| US4847190A (en) | Manufacturing process for silver halide photographic emulsion | |
| JPS59154437A (en) | Apparatus for producing silver halide photographic emulsion | |
| JPH08254773A (en) | Preparation of silver halide emulsion |