JPH0248481B2 - - Google Patents

Description

[Detailed description of the invention] [Industrial application field] The present invention relates to spheroidized iodine.

[Prior Art and Problems] In general, various meltable substances are handled in their own unique states, such as by cooling and solidifying the melt into flakes, sublimated crystals, lumps, powders, granules, etc. It is being said. Among these, granulated products have advantages such as convenience in packaging and handling during use, and uniform reaction. Conventionally, granulation is performed by cooling and solidifying on a rotating disk or cylinder to form flakes, or cooling and solidifying into lumps, and then crushing them to form granules.

However, when handling iodine using these general methods, iodine is corrosive and sublimes, so
The equipment and operations are relatively complex and can easily lead to difficulties. Furthermore, some of the iodine that has sublimated and become powder adheres to the surface of the finished granular product, causing minute irregularities on the surface, lowering the product value and causing caking after packaging. There are drawbacks such as.

[Means for Solving the Problems] As a result of repeated studies in order to solve the problems of the prior art, the present inventor has developed a spherical iodine particle with a particle size of 0.3 to 5 mm that has a smooth surface with metallic luster. We have found that by using a chemical compound (hereinafter referred to as this product), extremely favorable results as described below can be obtained.

(1) The surface of this product has no powdered iodine attached to it and has a smooth surface with a metallic luster, so it has good fluidity and a small angle of repose, and can be supplied from a hopper etc. During this process, no crosslinking or clogging occurs.

In addition, if powdered iodine is attached as in conventional products, minute irregularities will occur on the surface, and the surface will not have a smooth metallic luster like this product.

(2) Since this product is spherical and has a smooth surface with a metallic luster, the surface area is small and the amount of sublimation from the surface is small, and the sublimated material may condense and adhere to the surface of the iodine granules. The occurrence of caking caused by Furthermore, since this product is a spherical body with a smooth surface, the contact area between the spherical bodies is small, which also contributes to prevention of caking.

In addition, if the particle size is 0.3 mm or less, a sufficient effect cannot be expected, and if the particle size is 5 mm or more, it becomes easy to crush during handling.

(3) Furthermore, there is less loss due to deviation as steam, leading to cost reduction. Furthermore, since the particle size is controlled to a nearly uniform particle size distribution, it does not dissolve rapidly and has a stable dissolution rate, compared to conventional flaky iodine.
The reaction is rate-limiting.

The above-described method of the present invention can be carried out using suitable equipment, and particularly preferred embodiments will be described below with reference to the accompanying drawings.

This product can be suitably manufactured by the following method.

That is, iodine is melted and continuously blown out from a nozzle to form droplets, and as the droplets disperse and fall, an insoluble liquid having a boiling point lower than the melting point of iodine is sprayed in the form of a spray, thereby forming the droplets. Cool and solidify. According to this method, iodine, which is corrosive and sublimable, can be smoothly and advantageously spheroidized without requiring complicated equipment and operations. Furthermore, the obtained spheroidized product is a new type of spherical product with a smooth surface with a metallic luster, does not have iodine partially sublimed and powdered on the particle surface, and does not cause caking even after packaging. It is something.

When using this method, iodine is blown out as droplets from a nozzle and falls, and at the same time, a sprayed liquid is sprayed as a coolant to rapidly cool and solidify. This prevents iodine from escaping, increasing efficiency and reducing the formation of fine powder that can cause product caking. It is also important that the atomized liquid as a coolant is a non-dissolving liquid with a boiling point lower than the melting point of iodine. Non-dissolving means that the atomized liquid does not dissolve the iodine;
Additionally, the atomized liquid is chosen to be inert and not react with iodine (eg water). Thus, the atomized fine liquid as a coolant contacts the surface of the iodine droplets and undergoes heat exchange thereon. That is, iodine is cooled and solidified in the form of droplets, and the atomized liquid comes into contact with a substance having a boiling point higher than its own, obtains latent heat of vaporization, evaporates into gas, and is easily discharged from the system. For this reason, spheroidized iodine products include
No atomized liquid is mixed in as a coolant.

The method described above may be carried out using any suitable apparatus, and particularly preferred embodiments will be described below with reference to the accompanying drawings.

That is, the attached drawings show a droplet forming nozzle 2 for forming droplets of molten iodine and introducing the droplets into the main body 1, and a coolant consisting of an insoluble inert liquid such as water, in the apparatus body 1 surrounding the contact zone. A manufacturing apparatus for the present product is illustrated, which is provided with a spray nozzle 3 for introducing atomized water into the main body 1, and further provided with an outlet 4 for taking out the product and an outlet 5 for discharging the evaporated product of the coolant.

First, the above method will be explained in detail with reference to FIG.
A droplet forming nozzle 2 connected via a conduit 7 is placed at the top of the main body 1 of the apparatus to form droplets of iodine.
The coolant injection nozzle 3 is attached horizontally to the side wall of the apparatus main body 1 at a position where the iodine droplets change from a continuous state to a discontinuous state below the droplet formation nozzle 2, and the supply pipe 8 is A coolant is supplied by connecting to a pump 9, and a discontinuous iodine mist coolant is sprayed and cooled to form a spherical sublimable object.

A device main body 1 facing the coolant injection nozzle 3
An exhaust port may be opened at a location located below the nozzle 3 on the side wall of the exhaust gas pipe 10, and an exhaust gas pipe 10 may be connected to the exhaust gas recovery tower (not shown) to absorb the exhaust gas.

Also, an air supply pipe 11 may be installed below the device main body 1 to constantly supply air, or an outlet 4 such as a conveyor may be installed below the device main body 1 to prevent falling spherical objects. It is also possible to receive the iodine and send it to a receiving tank 12 installed below the outlet 4.

Next, the above method will be explained in detail with reference to FIG.

That is, the apparatus main body 1 is installed so that the lower surface thereof faces into a receiving tank 12 filled with a cooling liquid 13 such as water. Then, the coolant injection nozzle 3 provided on the upper side of the apparatus main body 1 is installed diagonally downward, and further the coolant injection nozzle 3' is installed diagonally upward on the lower side of the apparatus main body 1,
The coolant injection nozzle 3 is connected to a branch supply pipe 8' branched from a supply pipe 8 connected to a pressure pump 9. In addition, there are guide and discharge ports 10 and 11 at the top and bottom of the device main body 1.
one of which is connected to the exhaust gas recovery tower and the other to an air supply source. Others are 1st
Since it is similar to the figure, the same reference numerals are given and the explanation will be omitted.

[Function] By converting iodine into a spheroid with a particle size of 0.3 to 5 mm and a smooth surface with metallic luster,
It prevents caking, reduces losses due to vapor escape, and stabilizes the dissolution rate.

[Example] Next, typical examples of the present invention will be described in more detail.

Example 1 According to Figure 1 of the attached drawings, iodine (melting point
113.5℃) into an atomized liquid with distilled water (boiling point 100℃)
A granulation method was carried out using

Melt 50 iodine from kettle 6, melt iodine (130
~150° C.) is dispersed and dropped as droplets from the nozzle 3 onto the upper center of the main body 1 through the conduit 7. The dropping rate of molten iodine is 5 kg/min, nozzle hole 1 mmφ
It is 150 pieces. The main body 1 is a cylinder made of vinyl chloride resin with a diameter of 400 mm and a size of 3 m. The main body 1 is a cylindrical cylinder made of vinyl chloride resin and has a diameter of 400 mm. Also,
At the bottom of the main body 1, an air supply pipe 11, a belt conveyor 4, and a product receiving tank 12 are provided. Meanwhile, distilled water is sprayed as a coolant from the spray nozzle 3 at a rate of 400 to 600 gr/min. 9 indicates a pressure pump. The spherical iodine thus obtained has a particle size of 0.3 to 5.
mm, and its particle size distribution is 7 to 32 meshes to 100
It was %. This spherical iodine has a smooth surface and metallic luster.

The angle of repose of this product obtained in this way is 32 degrees, and when it is packed in a 25 kg fiber drum container without causing any crosslinking or clogging when fed from the hopper, it will last for 6 months. However, no caking occurred and it was easy to take out.

[Comparative example] On the other hand, when using the conventional product, the angle of repose is
The temperature was 66°, and bridging, clogging, and caking occurred frequently. When the same packaged product as in Example 1 was stored for one month, caking occurred and the iodine could not be easily flowed out even if the container was tilted.

Example 2 According to FIG. 2 of the attached drawings, molten iodine is dripped from a dispersion nozzle, brought into counter-current or co-current contact with an atomized coolant for slow cooling, and then poured into a product receiving tank filled with coolant. A method of cooling and solidifying was conducted.

Melted iodine (130-150℃) is converted into droplets through nozzle 2.
The liquid is dispersed into droplets at the upper center of the main body 1. The dropping rate was 5 kg/min, and the nozzle holes were 1 mmφ x 150 pieces. The main body 1 is a cylinder made of vinyl chloride resin with a diameter of 400 mm and a diameter of 3 m.
It is led to an exhaust gas recovery tower (not shown). Also, main body 1
At the bottom, an air supply pipe 11 and a product receiving tank 12' are provided. Meanwhile, distilled water is sprayed as a coolant from the spray nozzle 3 or 3' at a rate of 300 to 500 gr/min. 9 indicates a pressure pump. In this way, the particle size
A spherical iodine product with a thickness of 0.5 to 3 mm and a metallic luster on the surface was obtained.

The product obtained by the method of Example 2 also has properties similar to those of Example 1.

[Effects of the Invention] The spheroidized iodine having a new form obtained by the method of the present invention has a smooth surface with metallic luster, and no finely powdered substance is attached to the particle surface. Since the contact surface between the spheroids is small, it exhibits an excellent effect of reducing the occurrence of caking. This characteristic is effective in improving the efficiency of handling operations, and also leads to the effect of reducing loss due to dissipation as steam. Furthermore,
It has a particle size of 0.3 to 5 mm and has a substantially uniform particle size distribution, and it is also recognized that it does not dissolve rapidly and has a stable dissolution rate.

[Brief explanation of the drawing]

The attached drawings are schematic diagrams for explaining an example of the method for producing spheroidized iodine according to the present invention, and FIG. 1 is a cross-sectional view of an apparatus for explaining Example 1, and FIG. FIG. 2 is a cross-sectional view of the device to be described. In addition, in the figure, 1 is the main body of the device, 2 is the droplet forming nozzle,
3 is an injection nozzle, 4 is a take-out port, and 5 is a discharge port.

Claims (1)

[Claims] 1 Particle size with a smooth surface with metallic luster
A spheroid of iodine with a size of 0.3 to 5 mm.