JPS5820202A - Purification apparatus by pulverization - Google Patents

Abstract

PURPOSE:To continuously carry out the supply purification, drying, grinding of a stock material and the taking-out of purified pulverized product, by successively carrying out the charge of a solvent, the stirring thereof, the supply of a stock solution, the discharge of the solvent, the grinding of a purified solid substance and the discharge of the ground purified substance. CONSTITUTION:A stock solution is quantitatively supplied from a pipe 6 by a fixed delivery pump 7 while a solvent poured into a hollow container 1 by a pressurizing apparatus 11 is stirred by a shaft 3' and a propeller 3. On the other hand, the waste liquid sump 13 is evacutaed by a vacuum pump 14 to store a waste liquid in said sump 13 and the pressure reduction of the waste liquid sump 13 is subsequently stopped. In the next stage, while pressure is reduced by the pump 14, a purified solid substance is ground by rotating the shaft 3' and the propeller 3 and, at the same time, the obtained purified powder is dried while air is sent from an air sending pipe 8. After the reduced pressure of the waste liquid sump 13 is restored, the powdery purified substance is taken out from a pipe 9. At last, a solvent is again poured from a pipe 10, after the propeller 3 is rotated, and the solvent is discharged to wash the hollow container 1.

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a powder refining device for refining powder.

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 below the liquid injection hole in the lowest communicating pipe, and the raw material powder is placed in a container equipped with a filtration filter. 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 led to the cooling part through the vapor rise passage, cooled in this cooling part, and the powder is washed with this cooled liquid before being discharged from the communication pipe. The powder is repeatedly purified 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 refining process. It is not possible to obtain the purification process from 1. to the drainage process in one step, and there is no stirring process. This method has the drawbacks of poor purification efficiency per fixed amount of cleaning liquid and large variations in purification.

In order to eliminate the drawbacks of the above-mentioned conventional examples, the present invention provides a hollow container with a filtration filter, a rotating blade on the upper part of the filtration filter, and an opening/closing means on the side wall of the hollow container on the upper part of the filtration filter. 1st. ° A second pipe, a third pipe provided on the side wall of the hollow container in contact with the upper part of the crystal filter, and a fourth pipe having an opening/closing means provided on the side wall of the hollow container below the filtration filter. and a fifth pipe installed at the bottom of the hollow container. A fixed volume pump connected to the second pipe supplies a fixed volume of the solutionized powdered raw material, and the rotating cocoon is rotated through the hollow container. The shaft is connected to the shirt shaft passing through the hole at the top, and by rotating the shaft with a motor, the powdered raw material is stirred, the refined solid content is crushed, and gas is blown through the first pipe to form the refined powder. A pressure pump is connected to the fourth pipe to supply a solvent for refining the powdered raw material, and a vacuum pump connected to the fifth pipe performs purification. The purpose is to provide raw material supply, purification, drying, pulverization, and refining without requiring assembly and preparation of equipment for each refinement.Hereinafter, Examples will be explained in detail with reference to the drawings.

FIG. 1 shows a schematic configuration diagram of a pulverization and purification apparatus according to an embodiment of the present invention, in which 1 is a hollow container, and 2 is a filter mounting part 1 that divides the inside of the hollow container L into upper and lower parts. 3 is a propeller attached to the tip of a shaft 3' inserted through a shaft insertion hole 4 provided at the top of the hollow container 1, and 5 is attached to the other end of the shaft 3'. A motor 6 is provided on the upper side wall of the hollow container 1, to which a constant volume pumper is connected, and a first tube 8 is provided on the upper 9 side wall of the hollow container i, and a first tube 8 is provided with an opening/closing means 6'. A second pipe 9 having an opening/closing means 9' is provided in contact with the upper part of the filter 2, and a third pipe 10 having an opening/closing means 9'.
is provided on the side wall of the hollow container 1 at the bottom of the filtration filter 2, is connected to a pressurizing device 11, and has an opening/closing means 10'; 12 is provided at the bottom of the hollow container 1, and is a waste liquid reservoir 13. A fifth pipe to which a vacuum pump 14 is connected and has an opening/closing means 12', and the hollow container 1 is not subject to chemical or physical modification such as corrosion, other reactions, or swelling due to the solvent used. First, it is made from a material that has sufficient physical strength to withstand changes in operating conditions from raw material solution supply to waste liquid and powder removal processes, has good sealing properties, and is resistant to gas and liquid leakage. These materials include various types of glass, stainless steel, copper, brass, and other metals,
Composite materials such as Teflon-lined metal can be used.

Further, when the pressurizing device 11 supplies a small amount of solvent and supplies the solvent at a constant rate, a constant volume pump can also be used, and a high pressure gas or pressurizer is usually used. Furthermore, it is desirable to use a cold trap between the waste liquid reservoir 13 and the vacuum pump 14, and electric cooling (from liquefaction to vaporization of Freon gas or utilization of the Beltier effect) is used to cool this cold trap, but dry ice or A cooling medium such as liquid nitrogen ice may also be used.

The operation of the powder refining apparatus of this embodiment configured as described above will be explained. First, the opening/closing means 9' of the third pipe 9 which is a powder extraction part and the opening/closing means 1 of the fifth pipe 12 which is a waste liquid part.
2' is closed, the opening means 10' of the fourth pipe 10 serving as the solvent inlet is opened, and the solvent is injected into the hollow container 1 using the pressurizing device 11. After injecting this solvent, the opening/closing means 10' is closed. Next, a fixed amount is supplied from the sixth pipe 6 which is the supply part of the motor 5, and after the supply, the opening/closing means ♂ is closed. Thereafter, the opening/closing means 12' of the fifth pipe 12 is opened, the pressure is reduced by the vacuum pump 14, and the waste liquid is stored in the waste liquid reservoir 13. After draining the liquid, open the connection between the vacuum pump 14 and the waste liquid reservoir 13, stop depressurizing the waste liquid reservoir, and
Close the opening/closing means 12'.

Thus solvent pupil, solvent stirring, solvent effluent °? The refined powder is washed every second time the operation is repeated.

12' is opened, and while the pressure is reduced by the vacuum pump 14, the shaft, the shaft 3', and the propeller 3 are rotated by the motor 5 to crush the purified solids. At the same time, the opening/closing means 8' of the second pipe 8, which is a blowing pipe, is opened to dry the refined powder while blowing air.

Next, the opening/closing means 1 of the connection part of the vacuum pump 14 is closed, the opening/closing means 1:3' of the waste liquid reservoir 13 is opened to release the reduced pressure, and the opening/closing means of the fifth pipe 12 which is the waste liquid part is opened. 12' is closed.Then, the opening/closing means d of the third tube 9, which is the powder extraction section, is opened, and the powdered purified product is taken out.
The opening/closing means s/, 91 of the tube 9 is closed. Finally, the solvent is again injected from the pipe 10 of i4, the propeller 3 is rotated, and then the solvent is discarded and the hollow container is washed.

In addition, the powder storage section 15 and the vacuum pump 16 are connected to the third pipe 9, which is the powder extraction section □, as shown in FIG.
When the opening/closing means 9' of the third pipe 9 is opened, the vacuum pump 1
The opening/closing means 16' of the vacuum pump 16 is opened to take out the powder, and after taking out the powder, the opening/closing means 16' of the vacuum pump 16 is closed, and the opening/closing means 15 of the powder storage section 15 is opened. All you have to do is open it. In addition, during drying, the gas sent from the second tube 8, which is a blower tube, is heated to improve the drying speed, and in order to prevent reactions such as oxidation of the powder, the gas is heated to increase the drying rate.
It is preferable to use an inert gas such as Furthermore, it is desirable to blow an unheated inert gas to the powdered purified product gas in order to prevent thermal reactions of the powder, including acid threat reactions. Furthermore, a porous film is interposed between the vacuum pump 16 and the powder storage section 15 shown in FIG. 2 to prevent powder from entering the vacuum pump 16.
1 The cold trap provided between the vacuum pump 14 and the waste liquid reservoir 130 is further provided with two holes that can be opened and closed freely, one is connected to a pressurizing device, the other is connected to a solvent storage part, and the waste liquid reservoir 13 is connected to the cold trap. The opening/closing means 12' of the fifth pipe 12 of the waste liquid reservoir 13 and the vacuum release part 13' are closed, and the waste liquid reservoir 13 is heated while being depressurized by the vacuum pump 14, and the cold trap is connected. Then, the reduced pressure opening section 13' is opened, and when the pressure returns to normal pressure, the reduced pressure opening section 13' is closed.

Next, the solvent stored in the cold trap is delivered to the solvent storage section. Through the above operations, the solvent can be used repeatedly.

As explained above, according to the present invention, by sequentially performing the injection of the solvent, stirring the solvent, supplying the raw material solution, discarding the solvent, pulverizing the purified solid, and taking out the powdered purified product,
Purified powder can be efficiently processed by -m operation, and more refined powder can be taken out by injecting the solvent, stirring the solvent, and turning over only the waste pile of solvent. I can ride it.

[Brief explanation of the drawing]

FIG. 1 is a schematic diagram of a pulverizing and refining apparatus according to one embodiment of the present invention, and FIG. 2 is a diagram of another embodiment of a part of FIG. 1. ' 1...Hollow container, 2...Filter, 3...Propeller, 3'...Shaft, 4-...Shaft insertion hole, 5
...Motor, 6..First pipe, 2..Constant displacement pump, 8..Second pipe, 9..Third pipe, 10..
4th pipe, 11...pressure device, 12...5th pipe,
6', 8', 9', 10', l2'... Opening/closing means, 13... Waste liquid reservoir, 14... Vacuum pump,
15...Powder storage section, "16...Vacuum pump. Patent applicant Rico Co., Ltd. -

Claims (1)

[Claims] a first tube having an opening/closing means provided on an upper side wall of the hollow container; a second pipe having an opening means provided on a side wall of the hollow container opposite to the pipe; a third pipe provided on a side wall of the hollow container in contact with an upper part of the filter; a fourth pipe having an opening/closing means provided at a lower part of the filtration filter on the side wall of the hollow container opposite to the third pipe; and a fifth pipe having an opening/closing means provided at the lowest part of the hollow container. In the pulverization and purification apparatus, a constant volume pump is connected to the first pipe to supply a constant volume of the powdered raw material as a solution, and the rotary blade is configured to fill the hole at the top of the hollow container. By rotating the shaft with a motor, the solution is stirred and the purified solids are pulverized, and gas is blown from the second pipe to dry the purified powder and dry the purified powder. The purified powder is taken out from the pipe, a pressure pump is connected to the fourth pipe to supply a solvent for refining the powdered raw material, and a vacuum pump is connected to the fifth pipe to perform the refining process. A pulverization purification device characterized by removing the subsequent waste liquid.