JPS588522A - Method and apparatus for refining powder - Google Patents

Abstract

PURPOSE:To carry out purification operation in good efficiency, by carrying out a raw material supply process, a washing solvent pour-in process, a stirring process, a drain process, a drying process, a grinding process and a powder take- out process on production line basis. CONSTITUTION:A raw material is supplied from a first port 5 and washed by a washing solvent poured in from a fourth port 8 while stirred by a propella 3 connected to a shaft 3'. After washing for a definite period, the washing solvent is discharged from a fifth port 9 provided to the bottom part of a hollow container 1. After the washing solvent is discharged, a heated gas is sent in from a second port 6 while the container 1 is evacuated through the fifth port 9 as well as the stock material is dried while stirred by the propella 3. In this case, when drying is carried out, the raw material is ground while stirred by the propeller 3. After this grinding is carried out for a definite period, a purified powder is taken out from a third port 7.

Description

[Detailed description of the invention] It's about location.

Conventionally, the Soxhlet extraction method has been known as a method for refining powder. In this method, raw material powder is placed in a container equipped with a filtration filter, connected to the lowest communicating pipe, one hole is provided in the direction f from the liquid injection hole of this lowest communicating pipe, and the lowest communicating pipe is A steam rising passage with another hole provided above is connected, a cooling part is provided above the hole above the steam rising passage, and a liquid part is provided below the hole below the steam rising passage. In the device, the liquid part is heated and the evaporated liquid is guided to the cooling part through the vapor rising passage, cooled in this cooling part, and the powder is washed with the cooled liquid and discharged from the communication pipe. The powder is repeatedly cleaned using a high-purity cleaning solution.

However, since this method is a batch method, it is necessary to perform powder supply, removal, and equipment assembly preparation for each purification process. Furthermore, since there is no stirring step, there is a drawback that the purification efficiency per fixed amount of washing liquid is low, and there is a large variation in purification.

In order to eliminate the drawbacks of the conventional example, the present invention is characterized in that - raw material supply process, cleaning solvent injection process, stirring process, draining process, drying process, pulverization process, and powder removal process are carried out in one step. The purpose of this method is to eliminate the need to assemble and prepare equipment for each purification process, and to achieve high purification efficiency per fixed amount of washing liquid by using a stirring process.In other words, to obtain the same purity, the amount of washing liquid supplied is smaller than with conventional methods. The purpose of the present invention is to provide a powder refining method and apparatus that can perform uniform refining without having to perform the following steps.

Hereinafter, embodiments will be described in detail with reference to the drawings.

The figure shows a schematic configuration of an apparatus according to an embodiment of the present invention, in which 1 is a hollow container, 2 is a filtration filter installed at a filter attachment part 1' that divides the interior of the hollow container 1 into upper and lower parts, and 3 S is a propeller provided at the tip of a shaft 3' inserted from a shaft insertion hole 4 provided at the top of a hollow container L;
is provided on the upper side wall of the hollow container 1, and an opening/closing means 5'
A first hole 6 having an opening/closing means 6' is provided in the side wall above the first hole 5, and a second hole 6 having an opening/closing means 6' is provided in the side wall of the hollow container 1 in contact with the upper part of the filter 2. A third hole 8 having an opening/closing means is provided on the side wall below the filtration filter 2, and a fourth hole 9 having an opening/closing means 8' is provided at the bottom of the hollow container 1 and has an opening/closing means 8'. The hollow container 1 is provided with a drainage hole having a means 9', and the hollow container 1 does not undergo chemical or physical modification such as corrosion or other reactions or swelling due to the solvent used, and can be operated from the powder supply to the powder removal process. Any material can be used as long as it maintains sufficient physical strength against changes in process conditions, has good sealing properties, and is resistant to gas-liquid leakage. These materials include metals such as brass and composite materials such as Teflon-coated metal.

In the apparatus of this embodiment configured in this way, the raw material is first supplied through the first hole 5, the cleaning solvent is injected through the fourth hole 8, and the cleaning solvent is stirred by the propeller 3 connected to the shaft 3'. do. After cleaning for a certain period of time, the cleaning solvent is discharged from the fifth hole 9 provided at the bottom of the hollow container 1. After discharging this cleaning solvent, heated gas is fed through the second hole 6 while reducing the pressure through the fifth hole 9, and the raw material is dried while being stirred by the propeller 3. Further, during this drying, the raw material is pulverized while being stirred by the propeller 3. After this dry pulverization is carried out for a certain period of time, the purified powder is taken out from the third hole.

As described above, by repeating each step, uniformly purified powder can be taken out. Further, in the above process, by repeating only the injection of the cleaning solvent after supplying the raw materials, stirring by a propeller, and discharge of the cleaning solvent, a more refined powder can be obtained.

Note that it is desirable to supply the raw material by reducing the pressure in the hollow container 1, and this pressure reduction can be performed through the fifth hole 9. Additionally, the cleaning solvent may be introduced under pressure.
- The inside of the hollow container 1 may be depressurized and injected. If the hollow container 1 is transparent, the liquid volume can be controlled visually, but it is also possible to detect and control the amount by installing a sensor (temperature, current, liquid pressure, etc.) at a desired position in the hollow container 1. . Further, variations in purification efficiency and accuracy are often caused by stirring, but this can be controlled by the rotation speed of the motor and the shape of the propeller 3. Furthermore, by draining the liquid from the fifth hole 9 under reduced pressure, the work can be carried out more quickly. In the drying process, gas is sent through the second hole 6 and the fifth
Drying is performed while reducing the pressure from the hole 9 of the powder.In order to improve the drying speed, it is desirable that the gas be heated, and in order to prevent the powder from liquefying, the gas should be heated.
It is desirable to use N2, etc., excluding O2. Furthermore, the crushing efficiency and accuracy during the crushing process can be controlled by the rotation speed of the shaft 3' by the motor and the shape of the propeller.In addition, in this process, the gas is not heated to prevent thermal reactions of the powder. Preferably inert.

Furthermore, the powder is taken out by blowing unheated inert gas through the second hole 6 while reducing the pressure through the third hole 7. Further, after the filter 2 has been used for a predetermined period of time, the filter plate attaching portion 1 of the hollow container 1 is removed and the filter 2 is replaced.

As explained above, according to the present invention, the raw material supply step,
By sequentially performing the cleaning solvent injection step, stirring step, draining step, drying step, pulverization step, and powder removal step, the purified powder can be efficiently processed in a circular operation, and the above steps can be carried out efficiently. In step 7, by repeating only the washing solvent injection step, stirring step, and draining step 7, more purified powder can be taken out. .

[Brief explanation of drawings]

The figure is a schematic configuration diagram of an apparatus according to an embodiment of the present invention. 1... Hollow container, 2... Filtration filter, 3... Propeller, 3... Shaft, 4... Shaft insertion hole,
5...First hole, 6...Second hole, 7...Third hole, 8...Fourth hole, 9...Fifth hole, 5', 6'
, 7', 8', 9'... opening/closing means. Patent applicant Rico Co., Ltd. −

Claims (3)

[Claims] (1) A filtration filter is provided inside, and the filtration filter has first, second, and third holes provided at the top of the filter, and fourth and fifth holes provided at the bottom of the filtration filter. , in a hollow container having a stirring blade provided above the filtration filter, a step of supplying the raw material from the first hole above the filtration filter, and a step of supplying the raw material from the fourth hole below the filtration filter; a cleaning solvent injection step, a stirring step using the stirring blade, a draining step of the post-cleaning solvent from the fifth hole below the filtration filter, and an air blowing step from the second hole above the filtration filter. A drying process by continuing the liquid draining process, a pulverizing process by continuing the stirring process in the liquid draining process and the drying process, and a powder extraction process from the third hole in contact with the upper part of the filtration filter are sequentially performed. A powder refining method characterized by: (2) The powder refining method according to claim 1, wherein in the step, the washing solvent injection step, the stirring step, and the post-washing solvent draining step are repeatedly performed in sequence. (3) a filter provided near the middle part of the hollow container;
A stirring blade provided at the upper part of the filter, a gas blowing hole having an opening/closing means provided on the upper side wall of the hollow container, and an opening/closing means provided opposite to the side wall below the gas blowing hole. a raw material supply hole, a powder extraction hole provided on a side wall in contact with the upper part of the filter, and a liquid injection hole having an opening/closing means provided on a side wall opposite to the powder extraction hole at the lower part of the filter. A powder refining device comprising: a drain hole having an opening/closing means provided at the bottom of the hollow container;