JPH02254339A - Apparatus for estimating evaporation residue in volatilizing refined material - Google Patents

Abstract

PURPOSE:To estimate an evaporation residue efficiently by arranging an inner cylinder holding a volatilizing refined material while an evaporation thereof is repeated being placed in a cylinder. CONSTITUTION:An evaporation dish with a specified weight of selenium material Se measured is inserted into a distillation inner cylinder at an electric furnace 1. A cooling water flows through a cooling jacket 3 and a vacuum pump 15 is operated to bleed air within a distillation cylinder 2 through a vacuum hose 14, purifying bottles 13 and 11 and a vacuum hose 10. Under such a condition, when the furnace 1 is heated, the material Se is evaporated to flow to the other end side and the material evaporated is cooled on an internal surface of a cylinder 2 cooled with the jacket 3 to solidify and accumulated in a tank 5. The material passing the cylinder 2 is caught with a glass wool 16 when passing through the purifying bottles 11 and 13 so as not to be released to the outside air. Moreover, upon the completion of the evaporation, the distillation inner cylinder is taken out of the cylinder 2 and the weight of an evaporation residue in a magnetic evaporation dish is measured. Thus, a ratio of the evaporation residue is estimated as impurities contained in the material Se.

Description

DETAILED DESCRIPTION OF THE INVENTION [Industrial Application Field] The present invention relates to a quantitative device for determining the amount of evaporation residue of a volatile refining material such as selenium (Se).

[Prior Art] Conventionally, when measuring the amount of evaporation residue as an impurity of a volatile (or evaporative) refining material, such as a selenium material, the selenium material is heated and evaporated, and then the amount of residue remaining is measured. This is done by

[Problem to be solved by the invention 1 However, in the conventional technology for measuring the amount of evaporation residue,
No specialized equipment had been developed, and it was not possible to efficiently measure the amount of evaporation residue of large amounts of materials.

The present invention has been made in view of the above circumstances, and it is an object of the present invention to provide an apparatus for quantifying the evaporation residue of an evaporative refining material, which can efficiently determine the amount of evaporation residue.

[Means for Solving the Problems] In order to achieve the above object, the present invention includes a cylindrical body with one end open, a gas suction means connected to the other end of the cylindrical body,
a heater that heats one end side of the same body; an inner cylinder that is inserted into and out of the cylindrical body in a portion heated by the heater and stores a volatile refining material; and an inner cylinder that is provided at the other end of the cylindrical body. It is equipped with a cooling means and a tank connected to the cylindrical body near the cooling means.

[Operation] In the present invention, one end side of the cylinder and the inner cylinder are heated by the heater, and the volatile refining material stored in the inner cylinder is evaporated. The evaporated material is then drawn by the gas suction means and moved to the other end of the cylinder, where it is cooled by the cooling means. Then, the evaporated material becomes solid again and falls into the tank. When the evaporation of the volatile refining material is completed, the inner cylinder is removed from the cylinder and the amount of evaporation residue remaining in the inner cylinder is measured. By repeating the above operations, the amount of evaporation residue of a large amount of volatile refining material can be efficiently measured. Further, since the evaporated material is returned to a solid state and stored in a tank, it is economically advantageous and there is no risk of harming the environment.

[Embodiment] Hereinafter, an embodiment of the present invention will be described with reference to FIGS. 1 and 2.

In FIG. 1, reference numeral 1 denotes a cylindrical electric furnace (heater) with one end open, and this electric furnace 1 includes, for example, a distillation column (cylindrical body) for distilling selenium material (volatile refining material).
2 is inserted.

As shown in FIG. 2, the distillation column 2 is made of quartz or stainless steel (for example, 5US304) and is formed into a cylindrical shape with one end open.
is inserted into and held in the electric furnace 1, and at that time,
The other end side portion is exposed from the electric furnace 1. A cooling jacket (cooling means) 3 is provided on the outer periphery of the other end of the distillation column 2 exposed from the electric furnace 1.

The cooling jacket 3 is formed into a cylindrical shape so that its outer circumference surrounds the distillation column 2, and at a symmetrical position on the outer circumference, there is an inlet for cooling water W that cools the outer circumference of the other end of the distillation column 2. 3a and an outlet 3b for the cooling water W are formed.

In addition, in the distillation column 2, on the left side of the cooling jacket 3,
A branch pipe 4 is connected adjacent to the cooling jacket 3.

This branch pipe 4 is formed in a cylindrical shape and is provided perpendicularly to the distillation column 2. A flange 4a is formed on the outer periphery of the distal end of this branch pipe 4, and a tank 5 having a flange 5a having a shape matching the flange 4a is connected to this flange 4a.

The tank 5 is a cylindrical container with one end provided with a flange 5a open and the other end closed, and a plurality of bolts 6 are connected to the flange 4a of the branch pipe 4 via the flange 5a. , are connected by nut 7.

In addition, the other end (the right end in the figure) of the distillation column 2 has a lid 8.
The lid 8 is designed to be closed with a distillation column 2.
An O-ring 9 is provided to maintain airtightness. An air extraction port 8a is formed in the center of the lid 8, and a first purification layer 11 is connected to the air bow extraction port 8a via a first vacuum hose IO. The first purification layer 11 is connected to the 20th purification layer via the second vacuum hose 12.
A purification bottle 13 is connected, and this second purification layer 3 is connected to a vacuum pump (gas suction means) 1 via a third vacuum hose 14.
It is connected to 5.

Inside the first purification layer 11 and the second purification layer 13,
The third vacuum hose 14 is filled with glass wool 16 as a purifying material, and the third vacuum hose 14 is a U-shaped tube 1 using a mercury column.
It is connected to 7.

In addition, a cylindrical distillation inner cylinder 18 with one end open is inserted into one end of the distillation column 2 so as to be freely removable. , a draft 19 for ventilation is provided. The above distillation inner cylinder 18
is made of quartz glass, hard glass or silicate glass.

Furthermore, in FIG. 1, the reference numeral 20 denotes a cooling water supply hose connected to the inlet 3a of the cooling jacket 3, and the reference numeral 21 denotes a drainage hose attached to the outlet 3b. 1 is a volatile refining material, which is a selenium material in a magnetic evaporation dish 22 inserted into the distillation inner cylinder 18 for the purpose of checking the amount of evaporation residue.

In the selenium material evaporation residue quantitative determination apparatus configured as described above, one end of the distillation column 2 is inserted into the electric furnace 1 with the tank 5 facing downward. In this state, from the left side of the electric furnace 1, the distillation inner cylinder 18 into which the magnetic evaporation dish 22 containing a predetermined weight of selenium material Se is inserted is inserted into one end side of the distillation cylinder 2. Then, cooling water is poured into the cooling jacket 3, the vacuum pump 15 is operated, and the third vacuum hose 14, the second purification layer 13, and the second vacuum hose 12 are removed.
, first purification layer 11, first vacuum hose 10 and M8
The air inside the distillation column 2 is drawn out to the other end side through the distillation column 2. In this state, the electric furnace 1 is heated to a temperature of 470°C or more inside it.
The temperature should be 530°C.

Then, the selenium material Se is evaporated and flows to the other end, and on the inner surface of the distillation column 2 cooled by the cooling jacket 3, the evaporated material is cooled and solidified again, and falls and accumulates in the tank 5. . Moreover, the material that has passed through the distillation column 2 is captured by the glass wool 16 when passing through the first purification layer 11 and the second purification layer 13, and is not released into the outside air. When the evaporation is completed, the distillation inner column 18 is taken out from the distillation column 2, the magnetic evaporation dish 22 is taken out from the distillation inner column 18, and the weight of the evaporation residue remaining in the magnetic evaporation dish 22 is measured. As a result, the proportion of evaporation residues as impurities contained in the selenium material Se is determined. moreover,
To quantify the evaporation residue of another selenium material Se, the distillation inner column 18 into which the magnetic evaporation dish 22 containing the selenium material Se is inserted is subsequently inserted into the distillation column 2 and heated. Further, the amount of selenium material Se accumulated in the tank 5 can be predicted to reach a negative level depending on the number of inspections, so when the amount becomes full, it is taken out from the tank 5 and used as normal selenium material Se. Furthermore, the gas flow ■ drawn from the distillation column 2 is
The degree of vacuum changes depending on the degree of vacuum of the vacuum pump 15, and this degree of vacuum is accurately measured by the difference in the upper surface position of the mercury columns on the left and right sides of the U-shaped tube 2. Therefore, the degree of vacuum of the vacuum pump 15 is accurately adjusted while monitoring the mercury column.

According to the apparatus for quantifying the evaporation residue of a selenium material configured as described above, the evaporation residue ratio of a large amount of selenium material Se can be efficiently detected by evaporating the selenium material Se in multiple times. I can do it. Since the evaporated material is not released into the atmosphere, there is no danger of harming the environment, and since the evaporated material is returned to the tank 5 as a solid, it is extremely advantageous economically. .

Further, selenium material is sometimes used by being vapor-deposited on a transfer drum in a copying machine, and the evaporation residue that remains after being used for vapor deposition in this case corresponds to the evaporation residue from this device. Therefore, it is possible to conduct a practical inspection of evaporation residues, which is extremely useful.

In the above embodiment, an apparatus for quantifying the evaporation residue of selenium material Se is shown, but it goes without saying that the apparatus may also be used to quantify the evaporation residue of other volatile refining materials.

[Effects of the Invention] As explained above, according to the present invention, by repeatedly putting the inner cylinder containing the volatile refining material into the cylinder and evaporating it, a large amount of volatile refining material remains after evaporation. Able to quantify substances efficiently. In addition, the evaporated material is returned to solid form and stored in the tank, so
Not only is it economically advantageous, but it also has the remarkable effect of not causing any harm to the environment.

[Brief explanation of drawings]

Figures 1 and 2 are diagrams showing one embodiment of the present invention, in which Figure 1 is a configuration diagram of an apparatus for quantifying evaporation residue of selenium materials, Figure 2 is a detailed diagram of a distillation column, and Figure 3 is a diagram showing an example of the present invention. is the ITI in Figure 2
- It is an arrow view along the II line. l... Electric furnace (heater), 2... Distillation column (cylindrical body), 3... Cooling jacket (cooling means), 5...
... Tank, 15 ... Vacuum pump (gas suction means), 18 ... Distillation inner cylinder.

Claims (1)

[Claims] A cylinder with an open end, a gas suction means connected to the other end of the cylinder, a heater that heats one end of the cylinder, and a portion heated by the heater that can freely enter and exit the cylinder. The method is characterized by comprising: an inner cylinder inserted into the cylinder for storing a volatile refining material; a cooling means provided at the other end of the cylinder; and a tank connected to the cylinder near the cooling means. A device for quantifying evaporation residues in volatile smelting materials.