JPH08146543A - Method and device for manufacturing silver halide compound photographic emulsion - Google Patents

Abstract

PURPOSE: To provide a pump and motor having a wide feed liquid flow range, low pulsation, no flow variation at feeding liquid for a long time, and capable of feeding halide solution and silver nitrate solution while precisely metering so as to avoid waste. CONSTITUTION: Silver nitrate solution 14 and halide solution 15 are prepared in respective preparation tanks 16a, 16b, pipings are connected from the bottoms of the preparation tanks 16 to respective helical screw, type pumps 18 through stop valves 17, the discharge parts of the pumps are connected to respective three way valves 19, one of the three way valves 19 is connected to a settling vessel 20 receiving colloidal water solution, the other is connected to a circulating route 24 to the preparation tank, and further the circulating routes are connected to measuring vessels 25 having electronic balances through valves 23. The helical screw type pump 18 is constructed so as to have the discharge quantity of 50 ml/min - 10 litre/min and metering accuracy of 5--50ml/min by speed control of a vector inverter motor, and it is the solution pump of low pulsation and good repeatability.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method and an apparatus for producing a silver halide emulsion, and particularly to precisely measure raw material solutions (silver nitrate solution, halogen salt solution) for producing a silver halide photographic emulsion into a precipitation container without waste. The present invention relates to a method and an apparatus for sending a liquid.

[0002]

2. Description of the Related Art As a process control method and apparatus for producing a silver halide emulsion, a method and apparatus for maintaining a desired pAg is disclosed in U.S. Pat. No. 3,821,002 in which a gear pump and an electromagnetic flow meter are combined. A method and an apparatus for feeding a raw material solution into a precipitation container while controlling the liquid flow rate are disclosed. Journal of the Photographic Society of Japan, Volume 30, No. 2, 29 to 32.
The page also describes the use of gear pumps and plunger pumps.

Further, US Pat. No. 4,031,912 discloses a liquid feeding method and apparatus using a blanker pump.

[0004]

However, since both the gear pump and the plunger pump have a narrow liquid-feeding flow rate range, the working volume of the raw material solution in the production of the silver halide emulsion is, for example, 10 liters or more. It is in the range of up to 500 liters, and in practice, it is necessary to keep the accuracy of metering and feeding the raw material solution at 5 to 50 ml / min. In that case, several pumps with different feeding flow rate ranges are installed and used. It was necessary to select the pump according to the liquid flow rate.

Further, a gear pump can be used for a gelatin-containing solution, but it is unsuitable for a silver nitrate solution because of its poor lubricity and abrasion and the like.
No., p. 30. Further, the plunger pump has a large pulsation of the liquid supply flow rate, and it is necessary to install a pulsation preventive device in the middle of the liquid supply system. Furthermore, in the gear pump, the liquid supply flow rate may change due to pressure fluctuations in the liquid supply system. It is difficult to send the raw material solution at a stable flow rate. Further, when the plunger pump and the gear pump are used for a long period of time, metal silver is deposited on the drive part and the seal part, which tends to cause remarkable fluctuations in the liquid supply flow rate. If an electromagnetic flow meter is used, 100
10 liters / mi from low flow rate range such as ml / min
It is difficult to obtain good reproducibility with a single electromagnetic flowmeter for measuring the liquid flow rate in a wide flow range of n, and the improved system is complicated and prone to failure, resulting in stable manufacturing. It was difficult to achieve.

The object of the present invention is to solve the above problems, to have a wide metering and liquid feeding range, and to stably and reproducibly measure and feed a halogen salt solution and a silver nitrate solution with a low pulsation and without long-term flow rate fluctuations. It is to provide a pump, a motor, and a system for weighing and verifying the flow rate of a liquid.

[0007]

The above object of the present invention is to provide a method for producing a silver halide photographic emulsion in which a silver nitrate solution and a halogen salt solution are reacted in a precipitation vessel in which a colloidal solution is present. A method for producing a silver halide photographic emulsion, wherein a halogen salt solution is precisely metered and fed by a helical screw type pump driven by a vector inverter motor.

[0008] Verification verification of the liquid flow rate value of a helical screw type pump driven by a vector inverter motor, which carries out precision metering of the silver nitrate solution and the halogen salt solution,
2. The method for producing a silver halide photographic emulsion according to claim 1, which is carried out periodically by using an electronic balance by automatically switching the flow paths. In a silver halide photographic emulsion manufacturing apparatus equipped with a reaction apparatus for a silver nitrate solution and a halogen salt solution in a precipitation vessel in which a colloidal solution is present, the means for precisely measuring and feeding the silver nitrate solution and the halogen salt solution is a vector inverter. It is composed of a motor-driven helical screw type pump, the material of the rotary rotor of the pump is SUS316L or titanium, and the material of the fixed stator is made of Hypalon. Vaseline is sealed in the joint between the rotary rotor and the drive shaft. An apparatus for producing a silver halide photographic emulsion, characterized in that an ethylene propylene trimer sheet is coated on the outside, a double mechanical seal is applied, and a fixed stator and a rotating rotor are installed vertically.

Is achieved by

The helical screw pump in the present invention is, for example, a mohno pump manufactured by Hyojin Kikai Co., Ltd.
In general, the one used is as shown in FIG. 2, and the sectional view of the pump is a fixed stator 1 having a shape similar to a double helix as shown in FIG. 3 and a rotating rotor which slightly eccentrically rotates inside thereof. When the rotary rotor 2 is rotated about the eccentric shaft center through the drive shaft 5 and the universal joint 7, the rotary rotor 2 reciprocates up and down while rotating inside the fixed stator 1, and The solution entered from the inflow port from the solution preparation tank is sent to the discharge part 4. The rotational force of the rotary rotor 2 can be precisely measured in a wide range of arbitrary liquid supply flow rate by using a vector inverter motor as a drive motor and precisely changing the rotational speed between high speed and low speed.

Further, the accuracy of measuring the flow rate of the liquid fed by the pump is such that the raw material solution is not being fed into the precipitation container, and the weighing valve having the electronic balance 21 is regularly provided by the switching valve 23 in the circulation path 24. It is possible to carry out a guarantee test by sending the solution into 25 and weighing it. Furthermore, by installing the fixed stator and the rotating rotor vertically, the adjusted raw material solution can be injected without waste.

In the helical screw type pump of the present invention, as shown in FIG. 3, the rotary rotor 2 is made of SUS31 as a liquid contact member that comes into contact with a silver nitrate solution and a halogen salt solution to be supplied.
6L or titanium, the fixed stator part 1 is made of Hypalon (product name of DuPont, USA), the vaseline is sealed in the universal joint part 7 of the rotary rotor 2 and the drive shaft 5, and the outside thereof is ethylene propylene trimer ( Common name EP
A sheet 9 (referred to as T) is used to prevent the metal powder generated in the universal joint portion 7 from flowing out. The inside of the universal joint part 7 is lubricated by petrolatum. This prevents contact with each raw material solution, that is, silver nitrate solution or halogen salt solution, and the seal between the power transmission rotary shaft 6 and the liquid contact part is a double mechanical seal 1.
As shown in FIG. 2, ion exchange water or distilled water as seal water 11 is passed through the seal water inlet 12 to the seal water outlet 13 at a pressure of 5 KPa to 100 KPa as shown in FIG. ing.

[0013]

EXAMPLE An example in which the helical screw pump of the present invention was used in a method and apparatus for producing a silver halide emulsion,
This will be described with reference to FIG. The silver nitrate solution 14 and the halogen salt solution 15 are adjusted to 50 liters by the respective preparation tanks 16a and 16b, and piped from the bottom of the preparation tank 16 to the respective helical screw type pumps 18a and 18b through the stop valves 17a and 17b. The discharge part 4 of each pump is connected to three-way valves 19a and 19b, one of the three-way valves to the precipitation container 20 containing the colloidal aqueous solution, and the other to the circulation paths 24a and 24b to the preparation tanks 16a and 16b. It is connected. As described above, the structures of the helical screw type pumps 18a and 18b are such that the discharge amount is 50 ml / min to 10 liters / min, the measurement accuracy is 5 ml / min to 50 ml / min, and the discharge pressure is 10K by controlling the rotation speed of the vector inverter motor.
It is a liquid delivery metering pump having Pa to 200 KPa, low pulsation and good reproducibility in a wide flow rate range, and by using a vector inverter motor for its drive, precise control can be performed from low rotation to high rotation. Add the silver nitrate solution and the halogen salt solution to the precipitation vessel and send them until the solution is sent.
The reactor is circulated in 6a and 16b, and the reactor is Japanese Patent Publication Sho 55.
A precipitation vessel having a mixer as disclosed in Japanese Patent Application Laid-Open No. -10545, and by using the helical screw type pump and a vectoron inverter in combination, a precise flow rate control can be performed stably and reproducibly to produce a silver halide emulsion. I can.

As a verification guarantee of the liquid flow rate of a helical screw type pump driven by a vector inverter motor, which precisely feeds a silver nitrate solution and a halogen salt solution,
Circulation paths 24a, 24b to the liquid preparation tanks 16a, 16b
It is possible to automatically switch the flow path to and to feed the solution to the weighing containers 25a and 25b through 23a and 23b, and to perform periodical verification by the electronic balances 21a and 21b.

[0015]

【The invention's effect】

(1) According to the method and apparatus for producing a silver halide emulsion of the present invention, in a conventional pump addition system, foreign matter such as a metal is deposited to cause flow fluctuation in about 10 hours of use. Precipitates did not occur even after continuous use for about 10 hours and 22 days a day, and stable and precise flow rate liquid feeding was possible.

(2) Since the liquid feed flow rate can be arbitrarily increased or decreased without using a liquid feed flow detector such as an electromagnetic flow meter, the raw material solution can be fed by a single pump in a wide liquid feed flow range. Equipment costs and construction costs have been greatly reduced. (3) The equipment is compact and can be installed in a narrow space.

[Brief description of drawings]

FIG. 1 is a flow sheet of a method and an apparatus for producing a silver halide emulsion of the present invention.

FIG. 2 is an external view of the helical screw pump of the present invention.

FIG. 3 is a vertical sectional view of the helical screw pump of the present invention.

[Explanation of symbols]

1 Fixed Stator 2 Rotating Rotor 3 Inlet from Liquid Conditioning Tank 4 Discharge Port 5 Drive Shaft 6 Power Transmission Rotating Shaft 7 Universal Joint 9 EPT Cover 10 Double Mechanical Seal 11 Seal Water 12 Seal Water Inlet 13 Seal Water Outlet 14 Silver Nitrate Solution 15 Halogen salt solution 16a, 16b Preparation tank 17a, 17b Stop valve 18a, 18b Vector inverter motor driven helical screw pump 19a, 19b Three-way valve 20 Precipitation vessel 21a, 21b Electronic balance 22a, 22b Filter 23a, 23b Switching valve 24a, 24b Circulation system 25a, 25b Weighing container

Claims (3)

[Claims] 1. In a precipitation vessel in which a colloidal solution is present,
In the method for producing a silver halide photographic emulsion in which a silver nitrate solution and a halogen salt solution are reacted, the silver nitrate solution and the halogen salt solution are added by precision metering and feeding by a helical screw type pump driven by a vector inverter motor. A method for producing a silver halide photographic emulsion. 2. An electronic balance is used to automatically certify the solution flow rate of a helical screw type pump driven by a vector inverter motor for precisely measuring and delivering the silver nitrate solution and the halogen salt solution using an electronic balance. The method for producing a silver halide photographic emulsion according to claim 1, which is carried out periodically. 3. In a precipitation vessel in which a colloidal solution is present,
In a silver halide photographic emulsion manufacturing apparatus equipped with a reaction device of a silver nitrate solution and a halogen salt solution, the means for precisely measuring and feeding the silver nitrate solution and the halogen salt solution comprises a helical screw type pump driven by a vector inverter motor, The material of the rotary rotor of the pump is made of SUS316L or titanium, the material of the fixed stator is made of Hypalon, Vaseline is sealed in the joint between the rotary rotor and the drive shaft, and the outside is covered with ethylene propylene trimer sheet. An apparatus for producing a silver halide photographic emulsion, wherein a double mechanical seal is applied and a fixed stator and a rotating rotor are installed vertically.