JP6935301B2 - Coated particles for monohalogenoamine production - Google Patents

Description

The present invention relates to a coating particle group for monohalogenoamine production and a method for producing a coating particle group for monohalogenoamine production.

Chlorine-containing compounds are used as chlorine-based sterilizers in a wide range of fields such as foodstuffs, medical equipment, kitchen utensils, daily equipment, indoor cleaning sterilization, sterilization of human bodies and animals and plants, sterilization of bathtubs and pools, and sterilization. It is used for.
Hypochlorous acid is the most widely used chlorine-based disinfectant. On the other hand, there is a problem that the concentration of hypochlorous acid is lowered by the decomposition reaction by an organic substance, and the bactericidal effect is lowered because the pH is alkaline. Therefore, we focused on monochloramine, which is a type of bound chlorine, as a fungicide to replace hypochlorous acid.
Compared with hypochlorous acid, monochlorolamin has advantages such as being less likely to react with organic substances and having an excellent durability of effect, being less likely to corrode metal materials, having high persistence, and acting on biofilms. On the other hand, since the storage stability at a high concentration is poor, it is generally used by so-called time-of-use preparation, which is generated each time it is used.
Monochlorolamin is obtained by reacting chlorine or hypochlorous acid with ammonia.

Patent Document 1 describes that in a method for synthesizing monochloroamine by reacting an ammonium chloride solution with a sodium hypochlorite solution, the sodium hypochlorite solution is preliminarily made alkaline with an inorganic base and is contained in a reaction medium. A method of setting the ratio of the concentration of ammonium chloride to the concentration of sodium hypochlorite in the reaction medium to 1 to 1.5 is described.

In the examples of Patent Document 2, a protozoan in a water purification tank for circulating water purification, which synthesizes monochloroamine by directly injecting ammonia water or ammonium salt water and sodium hypochlorite solution into the source tank using a medicinal pump. The inactivation method is disclosed.

Japanese Unexamined Patent Publication No. 2004-155651 Japanese Unexamined Patent Publication No. 2008-264678

In Patent Document 1 and Patent Document 2, monochlorolamin is generated from a liquid raw material, and in order to prepare and use it as a disinfectant or disinfectant at the time of use, a huge raw material storage space and complicated operations must be accepted. ..
When generating monohalogenoamines such as monochloroamine, a compound that releases hypohalous acid and / or hypohalogenate ion when dissolved in water (hereinafter, also referred to as a halogen agent), a solid ammonium salt, and a solid It is necessary to add three kinds of alkaline agents individually to water to generate monohalogenoamine, but adding three kinds individually requires complicated operations from the user's side and is convenient. Is bad. Further, when the three types are mixed and made into one agent, the halogen agent and the solid ammonium salt generate rapid heat generation due to the oxidation / reduction reaction, so that both need to be formulated separately. On the other hand, when a solid ammonium salt and a solid alkaline agent are mixed to form a single agent, ammonia is generated by the neutralization reaction, which poses a problem.

In the present invention, by unifying a solid ammonium salt and a solid alkaline agent, monohalogenoamine can be easily synthesized in combination with a halogen agent, the dissolution rate in water is good, and the ammonia odor of the agent can be eliminated. Provided are a coating particle group for producing monohalogenoamine and a method for producing a coating particle group for producing monohalogenoamine.

In the present invention, at least a part of the particles of the (A) solid ammonium salt (hereinafter, also referred to as the (A) component) is coated with the (C) water-soluble binder (hereinafter, also referred to as the (C) component). Further, the present invention relates to a group of coated particles for producing monohalogenoamine, which are coated particles in which particles of a solid alkaline agent (hereinafter, also referred to as component (B)) are attached to a component (C) coated with the component (A).

The present invention also relates to a method for producing a coated particle group for producing monohalogenoamine, which comprises the following steps (1) and (2).
Step (1): Particles of (A) solid ammonium salt (hereinafter, also referred to as (A) component) and (C) water-soluble binder (hereinafter, also referred to as (C) component) are mixed, and at least one of the surfaces is mixed. Step of obtaining a coated particle group (1) composed of particles of the component (A) whose part is coated with the component (C) Step (2): The coated particle group (1) and (B) obtained in the step (1). The particles of the solid alkaline agent (hereinafter, also referred to as the component (B)) are mixed, and the component (C) coated with the component (A) of the coated particle group (1) obtained in the step (1) is mixed with the component (B). Step of obtaining coated particle group (2) composed of particles to which component particles are attached

According to the present invention, by unifying a solid ammonium salt and a solid alkaline agent, monohalogenoamine can be easily synthesized in combination with a halogen agent, the dissolution rate in water is good, and the agent ammonia. Provided are a coating particle group for producing monohalogenoamine and a method for producing a coating particle group for producing monohalogenoamine that suppress odor.

Electron micrograph of the surface of ammonium chloride salt particles, which is the component (A) Electron micrograph of the particle surface of the coated particle group (2) produced in Example 1

<Coated particle group for monohalogenoamine production>
In the coated particle group for producing monohalogenoamine of the present invention, at least a part of the particles of the component (A) is coated with the component (C), and the component (C) coated with the component (A) is further coated with the component (B). ) A group of coated particles composed of coated particles to which the particles of the component are attached.

[(A) component]
The component (A) is a solid ammonium salt. The component (A) is a raw material for the synthesis of monohalogenoamine. As the component (A), an ammonium salt comprising ammonium ions (NH 4 ^₊₎ (hereinafter, the inorganic referred ammonium salts) and organic ammonium salts containing ions (hereinafter, referred to as organic ammonium salts). An organic ammonium ion is an ion in which the hydrogen atom of the ammonium ion is replaced with a group containing carbon. The component (A) is preferably an inorganic ammonium salt from the viewpoint of increasing the monohalogenoamine production rate. The component (A) is preferably a solid ammonium salt containing ammonium ions from the viewpoint of increasing the monohalogenoamine production rate.

Inorganic ammonium salts include ammonium chloride, ammonium sulfate, triammonium phosphate, ammonium dihydrogen phosphate, ammonium nitrate, ammonium bromide, ammonium iodide, ammonium carbonate, ammonium hydrogencarbonate, ammonium oxalate, ammonium acetate, ammonium lactate, and citrus. Ammonium acid is mentioned.

Examples of the organic ammonium salt include a primary ammonium salt and a secondary ammonium salt. Here, the primary ammonium salt is one in which one of the hydrogen atoms of ammonium ion is substituted with a group containing carbon, and the secondary ammonium salt is one in which two hydrogen atoms of ammonium ion are substituted with a group containing carbon. Say.

The component (A) is preferably ammonium chloride, ammonium sulfate, triammonium phosphate, ammonium dihydrogen phosphate, ammonium nitrate, ammonium bromide, ammonium iodide, ammonium carbonate and hydrogen carbonate from the viewpoint of increasing the monohalogenoamine production rate. It is a compound selected from ammonium.
The component (A) is more preferably a compound selected from ammonium chloride, ammonium sulfate, triammonium phosphate, ammonium dihydrogen phosphate, ammonium nitrate, ammonium carbonate and ammonium hydrogen carbonate from the viewpoint of increasing the monohalogenoamine production rate. ..
The component (A) is more preferably ammonium chloride from the viewpoint of increasing the monohalogenoamine production rate.

From the viewpoint of suppressing the decomposition of monohalogenoamine and increasing the production rate of monohalogenoamine, the counter ion of the component (A) is preferably chloride ion, sulfate ion, phosphate ion, hydrogen phosphate ion, or diphosphate. It is selected from hydrogen ion, nitrate ion, bromide ion, iodide ion, carbonate ion, hydrogen carbonate ion, oxalate ion, acetate ion, lactate ion, and citrate ion.
The counter ion of the component (A) is more preferably chloride ion, sulfate ion, phosphate ion, hydrogen phosphate ion, or phosphoric acid from the viewpoint of suppressing the decomposition of monohalogenoamine and increasing the production rate of monohalogenoamine. It is selected from dihydrogen ion, nitrate ion, bromide ion, iodide ion, carbonate ion, and hydrogen carbonate ion.
The counter ion of the component (A) is more preferably chloride ion, sulfate ion, phosphate ion, hydrogen phosphate ion, or phosphoric acid from the viewpoint of suppressing the decomposition of monohalogenoamine and increasing the production rate of monohalogenoamine. It is selected from dihydrogen ion, nitrate ion, carbonate ion, and hydrogen carbonate ion.
The counter ion of the component (A) is more preferably a chloride ion from the viewpoint of suppressing the decomposition of monohalogenoamine and increasing the production rate of monohalogenoamine. The component (A) is even more preferably an ammonium salt composed of ammonium ions and chloride ions, that is, ammonium chloride.

From the viewpoint of handleability and solubility, the average particle size of the particles of the component (A) is preferably 100 μm or more, more preferably 300 μm or more, still more preferably 500 μm or more, still more preferably 700 μm or more, still more preferably 800 μm. The above, preferably 5,000 μm or less, more preferably 3,000 μm or less, still more preferably 2,000 μm or less, still more preferably 1,800 μm or less, still more preferably 1,500 μm or less. The average particle size can be measured by using the method described in Examples.

[(B) component]
The component (B) is a solid alkaline agent. The component (B) serves as a monohalogenoamine decomposition inhibitor during the synthesis of monohalogenoamine. The component (B) is an alkali metal hydroxide, an alkaline earth metal hydroxide, an alkali metal silicate, an alkali metal oxide, an alkaline earth metal oxide, an alkali metal coal oxide, and an alkaline earth metal coal oxide. It is a solid alkaline agent selected from.

Examples of the alkali metal hydroxide as the component (B) include potassium hydroxide and sodium hydroxide from the viewpoint of suppressing the decomposition of monohalogenoamine and increasing the production rate of monohalogenoamine, and potassium hydroxide is preferable.
Examples of the alkaline earth metal hydroxide as the component (B) include calcium hydroxide and magnesium hydroxide from the viewpoint of suppressing the decomposition of monohalogenoamine and increasing the production rate of monohalogenoamine, and calcium hydroxide is preferable. Examples of the alkaline earth metal hydroxide include alkaline earth metal chloride hydroxides such as magnesium hydroxide hydroxide and calcium chloride.
Examples of the alkali metal silicate of the component (B) include sodium silicate and potassium silicate from the viewpoint of suppressing the decomposition of monohalogenoamine and increasing the production rate of monohalogenoamine, and sodium silicate is preferable. The sodium silicate is preferably sodium metasilicate.
Since the alkali metal oxide and the alkaline earth metal oxide react with water to become an alkali metal hydroxide or an alkaline earth metal hydroxide, they can be used as the component (B) in the present invention. Examples of the alkali metal oxide include sodium oxide and potassium oxide. Examples of the alkaline earth metal oxide include magnesium oxide and calcium oxide.
Examples of the alkali metal coal oxide of the component (B) include sodium carbonate and potassium carbonate from the viewpoint of suppressing the decomposition of monohalogenoamine and increasing the production rate of monohalogenoamine, and sodium carbonate is preferable.
Examples of the alkaline earth metal coal oxide as the component (B) include calcium carbonate and magnesium carbonate from the viewpoint of suppressing the decomposition of monohalogenoamine and increasing the production rate of monohalogenoamine, and calcium carbonate is preferable.
As the component (B), an alkaline earth metal hydroxide is preferable, and calcium hydroxide is more preferable, from the viewpoint of suppressing the decomposition of monohalogenoamine and increasing the production rate of monohalogenoamine.

The average particle size of the particles of the component (B) is preferably 5 μm or more, more preferably 10 μm or more, and preferably 50 μm or less, more preferably 30 μm or less, from the viewpoint of coating property and solubility in the component (A). Is. The average particle size can be measured by using a laser diffraction / scattering type particle size distribution measuring device (for example, LA-920 manufactured by HORIBA).

[(C) component]
The component (C) is a water-soluble binder. The component (C) is such that at least a part of the particles of the component (A) is coated with the component (C) to reduce the direct contact between the particles of the component (B) and the component (A) to be subsequently adhered. Therefore, it is a component that suppresses the generation of ammonia due to the neutralization reaction. That is, the component (C) functions as a water-soluble coating agent.
The component (C) is preferably a water-soluble polymer binder from the viewpoint of solubility in water and coating property.
Specific examples of the component (C) include polyethylene glycol, polypropylene glycol, polyoxyethylene alkyl ether, polyoxyethylene phenol ether and the like from the viewpoint of solubility in water and coating property, and polyethylene glycol, polypropylene glycol and the like. One or more selected from polyoxyethylene alkyl ether is preferable, one or more selected from polyethylene glycol and polypropylene glycol is more preferable, and polyethylene glycol is further preferable.

The number average molecular weight of the component (C) is preferably 4,000 or more, more preferably 6,000 or more, and preferably 20,000 or less, more preferably 13,000 or less, from the viewpoint of granule strength and solubility. Is.
The number average molecular weight of the component (C) is a value measured by a gel permeation chromatography (GPC) method using polystyrene as a standard, and when the component (C) is polyethylene glycol, water / ethanol can be used as a solvent. ..

[Composition, other ingredients, etc.]
The coated particle group for producing monohalogenoamine of the present invention is a coated particle group for producing monohalogenoamine composed of particles containing the component (A), the component (B), and the component (C), and the component (A). This is an aggregate of particles having a structure in which at least a part of the particles of the component (C) is coated with the component (C), and the particles of the component (B) are attached to the component (C) coated with the component (A).
That is, in the coating particle group for producing monohalogenoamine of the present invention, the particles of the component (A), the first coating layer of the component (C) covering the surface of the particles of the component (A), and the first coating layer It is an aggregate of particles having a second coating layer composed of the component (B) formed above.
In the coated particle group for producing monohalogenoamine of the present invention, at least a part of the particles of the component (A) is coated with the component (C), and the component (C) coated with the component (A) is further coated with the component (B). ) Contains coated particles to which the particles of the component are attached. The coated particles are coated particles in which the component (B) is attached to the surface of the coated particles in which at least a part of the particles of the component (A) is coated with the component (C). The coated particle group for producing a monohalogenoamine of the present invention may contain particles other than the coated particles as long as the effects of the present invention are not impaired. For example, particles of the component (A), particles of the component (B), and particles coated with the component (C) may be included.

The average particle size of the coating particle group for producing monohalogenoamine of the present invention is preferably 100 μm or more, more preferably 500 μm or more, and preferably 5,000 μm or less, more preferably 3 from the viewpoint of handleability and solubility. It is 000 μm or less. The average particle size can be measured by using the method described in Examples.

The content of the component (A) in the coating particle group for producing monohalogenoamine of the present invention is preferably 30% by mass or more, more preferably 40% by mass or more, and further, from the viewpoint of the production rate and cost of monohalogenoamine. It is preferably 50% by mass or more, preferably 80% by mass or less, more preferably 70% by mass or less, still more preferably 60% by mass or less, still more preferably 55% by mass or less. The content of the component (A) in the coating particle group for monohalogenoamine production can be determined by the amount charged at the time of production, but can also be determined by a conventional method such as ion chromatography.

The content of the component (B) in the coating particle group for producing monohalogenoamine of the present invention is preferably 10% by mass or more, more preferably 20% by mass or more, and from the viewpoint of the production rate and cost of monohalogenoamine. It is preferably 50% by mass or less, more preferably 40% by mass or less. The content of the component (B) in the coating particle group for monohalogenoamine production can be determined by the amount charged at the time of production, but can also be determined by a conventional method such as elemental analysis.

The content of the component (C) in the coating particle group for producing monohalogenoamine of the present invention is preferably 10% by mass or more, from the viewpoint of storage stability, coating property to the component (B), and suppression of ammonia odor. It is preferably 15% by mass or more, preferably 40% by mass or less, more preferably 30% by mass or less, still more preferably 20% by mass or less, still more preferably 18% by mass or less. The content of the component (C) in the coating particle group for monohalogenoamine production can be determined by the amount charged at the time of production, but can also be determined by a conventional method such as liquid chromatography.

In the coating particle group for producing monohalogenoamine of the present invention, the mass ratio (A) / (B) of the content of the component (A) to the content of the component (B) is determined by the production rate of the monohalogenoamine and the handleability. From the viewpoint, it is preferably 0.5 or more, more preferably 1 or more, still more preferably 1.5 or more, and preferably 3 or less, more preferably 2.5 or less, still more preferably 2 or less.

In the coating particle group for producing monohalogenoamine of the present invention, the mass ratio (A) / (C) of the content of the component (A) to the content of the component (C) determines the storage stability and the component (B). From the viewpoint of coating property and suppression of ammonia odor, it is preferably 0.5 or more, more preferably 1 or more, further preferably 2 or more, still more preferably 2.7 or more, and preferably 6 or less, more preferably 5 or less. , More preferably 4 or less.

The total content of the components (A), (B) and (C) in the coating particle group for producing monohalogenoamine of the present invention is preferably from the viewpoint of the production rate, cost and handleability of monohalogenoamine. It is 70% by mass or more, more preferably 80% by mass or more, preferably 100% by mass or less, more preferably 90% by mass or less, and may be 100% by mass.

The coated particle group for producing monohalogenoamine of the present invention includes (D) a compound that releases hypochlorous acid and / or hypochlorous acid ion when dissolved in water (hereinafter referred to as component (D)) in water. Monohalogenoamine can be synthesized by mixing.
Examples of the component (D) include compounds selected from (D1) halogenated isocyanuric acid and salts thereof, (D2) halogenated hydantin and (D3) hypohalite.
When the component (D) is a solid compound, the coating particle group for producing a monohalogenoamine of the present invention can suppress heat generation when the particle group and the component (D) of the solid compound come into contact with each other. It is suitable from the viewpoint of sex.

Specific examples of (D1) halogenated isocyanuric acid and salts thereof include dichloroisocyanuric acid salts such as sodium dichloroisocyanuric acid and potassium dichloroisocyanuric acid, and bromoisocyanuric acid such as trichloroisocyanuric acid, sodium bromoisocyanurate and potassium bromoisocyanurate. Examples thereof include acid salts, dibromoisocyanuric acid, trichloroisocyanuric acid, and triiodoisocyanuric acid.
Specific examples of the halogenated hydantoin (D2) include chlorodimethyl hydantoin, dichlorodimethyl hydantoin, bromodimethyl hydantoin, dibromodimethyl hydantoin, iododimethyl hydantoin, diiododimethyl hydantoin, bromochlorodimethyl hydantoin, chloroiododimethyl hydantoin, and bromoiode. Dimethyl hydantoin can be mentioned.
Specific examples of the (D3) hypohalite include hypochlorous acid such as sodium hypochlorite, calcium hypochlorite, magnesium hypochlorite, calcium hypochlorous acid, and magnesium hypochlorous acid. Examples thereof include hypobrothates such as chlorate and sodium hypobromine, and hypoiodate such as sodium hypoiodate.

The component (D) is preferably a solid compound that releases hypochlorous acid and / or hypochlorite ions when dissolved in water. The component (D) is preferably chlorinated isocyanuric acid and a salt thereof, chlorinated hydantoin or hypochlorite.
From the viewpoint of increasing the production rate of monohalogenoamine, the component (D) is preferably sodium dichloroisocyanurate, potassium dichloroisocyanurate, trichloroisocyanuric acid, chlorodimethylhydranthin, dichlorodimethylhydranthin, sodium hypochlorite, hypochlorous acid. It is a compound selected from calcium chlorate, magnesium hypochlorite, calcium chloride hypochlorite, and magnesium hypochlorite.
The component (D) is more preferably a compound selected from sodium dichloroisocyanurate, trichloroisocyanuric acid, and calcium hypochlorite from the viewpoint of increasing the production rate of monohalogenoamine.
The component (D) is more preferably calcium hypochlorite from the viewpoint of increasing the production rate of monohalogenoamine.

The coating particle group for producing monohalogenoamine of the present invention may appropriately contain components other than the components (A) to (C) as long as the problems of the present invention can be solved. Other components may include fragrances, pigments, antifoaming agents, bulking agents, diluents and the like. These components may be contained in the coating particles.
Examples of the bulking agent or diluent include sulfates such as sodium sulfate and magnesium sulfate. By blending a bulking agent or a diluent, each component can be diluted and dispersed at an appropriate concentration to design an amount suitable for use.

<Production method of coated particle group for monohalogenoamine production>
The method for producing a coated particle group for producing monohalogenoamine of the present invention is a method for producing a coated particle group for producing monohalogenoamine, which comprises the following steps (1) and (2).
Step (1): A coated particle group (1) composed of particles of the component (A) in which at least a part of the surface is coated with the component (C) by mixing the particles of the component (A) and the component (C). Step to obtain Step (2): The coated particle group (1) obtained in step (1) and the particles of the component (B) are mixed, and (A) of the coated particle group (1) obtained in step (1). ) Step of obtaining a coated particle group (2) composed of particles of the component (B) attached to the component (C) coated with the component The method for producing the coated particle group for producing monohalogenoamine of the present invention is monohalogenoamine. The matters described in the coating particle group for production can be appropriately applied.

[Step (1)]
In step (1), the component (A) and the component (C) are mixed to obtain a coated particle group (1) composed of particles of the component (A) whose surface is at least partially coated with the component (C). It is a process.

The component (C) may be used by melting a part or all of it in advance, or it may be blended as a solid and heated and melted inside the mixer, but it is preferable to melt it in advance and use it.

In the step (1), when the component (A) and the component (C) are mixed to obtain the coated particle group (1), the content of the component (A) and the component (C) in the coated particle group (1) are obtained. The mass ratio (A) / (C) of the content of (A) is preferable from the viewpoint of uniformly covering the surface of the component (A) and suppressing heat generation when it comes into contact with sardine powder, and from the viewpoint of suppressing ammonia odor and solubility. Is 0.5 or more, more preferably 1 or more, still more preferably 2 or more, still more preferably 2.7 or more, and preferably 6 or less, more preferably 5 or less, still more preferably 4 or less. do.

In the step (1), a method of adding the component (C) to the component (A) is preferable from the viewpoint of the covering property of the component (A) by the component (C). The addition rate when the component (C) is melted in advance and added is preferably 1,000 g / min or less, more preferably 1,000 g / min or less, with respect to 100 g of the component (C), from the viewpoint of enhancing the coating uniformity of the component (A). Is 600 g / min or less, more preferably 200 g / min or less, still more preferably 150 g / min or less, still more preferably 100 g / min or less.

Mixers for mixing each component in step (1) include Henshell mixer (manufactured by Mitsui Mine Co., Ltd.), high-speed mixer (manufactured by Fukae Powtech Co., Ltd.), Nauter mixer (manufactured by Hosokawa Micron Co., Ltd.), and ribbon. Known mixers such as a mold mixer (manufactured by Tokuju Kosakusho Co., Ltd.), a V-type blender (manufactured by Dalton Co., Ltd.), and a bench kneader (manufactured by Irie Shokai Co., Ltd.) can be used. As the mixer, a high-speed mixer and a Henschel mixer are preferable from the viewpoint of the coating property of the component (C) on the component (A).

From the viewpoint of suppressing coarse-graining and crushing of raw materials during mixing, the Froude number of the granulator defined by the following formula is preferably set to 50 or less, more preferably 40 or less. It is more preferably 30 or less, further preferably 20 or less, and even more preferably 10 or less.

Froude number: Fr = V ² / (R × g)
V: Peripheral speed [m / s]
R: Radius from the center of rotation to the circumference of the rotating object [m]
g: Gravity acceleration [m / s ² ]
In a vertical or horizontal granulator equipped with a main wing or a crushing wing, V and R use the values of the main shaft, and in a Nauter mixer in which the stirring part draws a rotation and revolution trajectory, V and R are rotation stirring shafts. The value of is used.

In the step (1), the temperature at the time of mixing (jacket temperature of the mixer) is preferably 60 from the viewpoint of suppressing the solidification of the component (C) and uniformly coating the surface of the component (A) with the component (C). ° C. or higher, more preferably 70 ° C. or higher, and preferably 100 ° C. or lower, more preferably 90 ° C. or lower.

[Step (2)]
In the step (2), the coated particle group (1) obtained in the step (1) and the particles of the component (B) are mixed, and the coated particle group (1) (A) obtained in the step (1) is mixed. This is a step of obtaining a coated particle group (2) composed of particles in which particles of the component (B) are attached to the component (C) coated with the component.

In the step (2), when the coated particle group (1) obtained in the step (1) and the particles of the component (B) are mixed to obtain the coated particle group (2), the coating particle group (2) is included. The mass ratio (A) / (B) of the content of the component (A) to the content of the component (B) is from the viewpoint of the production rate of monohalogenoamine, storage stability, and suppression of heat generation when it comes into contact with sardine powder. , Preferably 0.5 or more, more preferably 1 or more, still more preferably 1.5 or more, and preferably 3 or less, more preferably 2.5 or less, still more preferably 2 or less.

In step (2), the mixer is the same as the mixer described in step (1).
Further, in the step (2), the temperature at the time of mixing (jacket temperature of the mixer) is preferably set from the viewpoint of suppressing the solidification of the component (C) and coating the surface of the coated particle group (1) with the component (B). It is 60 ° C. or higher, more preferably 70 ° C. or higher, and preferably 100 ° C. or lower, more preferably 90 ° C. or lower.
In the step (2), from the viewpoint of suppressing coarse-graining during mixing and crushing of the raw material, the Froude number of the granulator defined by the above formula is preferably set to 50 or less, preferably 40 or less. It is more preferably 30 or less, further preferably 20 or less, and even more preferably 10 or less.

[Step (3)]
From the viewpoint of reducing the odor of ammonia, the method for producing a coated particle group for producing a monohalogenoamine of the present invention preferably further includes the following step (3) after the step (2).
Step (3): A step of drying the coated particle group (2) obtained in the step (2).

In the step (3), the drying treatment is preferably vacuum drying, and the degree of vacuum is preferably 10 kPa abs or more, more preferably 15 kPa abs or more, and preferably 50 kPa abs or less, more preferably 40 kPa abs or less.
The drying time is preferably 1 hour or longer, more preferably 2 hours or longer, more preferably 5 hours or longer, more preferably 8 hours or longer, and preferably 24 hours or shorter, more preferably 16 hours or shorter.
The drying temperature is preferably 10 ° C. or higher, more preferably 20 ° C. or higher, further preferably 25 ° C. or higher, and preferably 70 ° C. or lower, more preferably 60 ° C. or lower, from the viewpoint of blocking suppression. More preferably, it is 55 ° C. or lower.

In step (3), normal pressure shelf drying can also be selected as the drying process. In this case, the drying time is preferably 1 hour or more, more preferably 2 hours or more, and preferably 24 hours or less, more preferably 16 hours or less. When shelf drying is performed, an open system is preferable.
The drying temperature is preferably 40 ° C. or higher, more preferably 50 ° C. or higher from the viewpoint of drying efficiency, and preferably 70 ° C. or lower, more preferably 60 ° C. or lower, still more preferably 55 ° C. from the viewpoint of blocking inhibition. It is as follows.

In the step (3), the drying treatment can also be selected by drying using a fluidized bed dryer. Examples of the fluidized bed dryer include SPIR-A-FLOW manufactured by FREUND. When the step (3) is performed using a fluidized bed dryer, the drying temperature is preferably 40 ° C. or higher, more preferably 50 ° C. or higher, and preferably 70 ° C. or lower from the viewpoint of blocking suppression. , More preferably 60 ° C. or lower, still more preferably 55 ° C. or lower.
From the viewpoint of drying efficiency, the amount of air blown is preferably 1 m ³ / min or more, more preferably 2 m ³ / min or more, still more preferably 3 m ³ / min or more, and preferably 10 m ³ / min or less.
The drying time is preferably 0.2 hours or more, more preferably 0.4 hours or more, and preferably 2 hours or less, more preferably 1 hour or less.

In the method for producing a coated particle group for producing a monohalogenoamine of the present invention, it is preferable to perform an aging treatment before the step (3). In particular, when vacuum drying is selected in the step (3), the storage stability is improved by the aging treatment. The aging treatment period is not particularly limited, but from the viewpoint of productivity, it is preferably within 1 month, more preferably within 2 weeks, most preferably within 1 week, and preferably 2 days or more, more preferably 3 More than a day.
The temperature is preferably 50 ° C. or lower, more preferably 40 ° C. or lower, and preferably 10 ° C. or higher, and may be room temperature. During aging, it is preferable to keep the seal closed from the viewpoint of suppressing moisture absorption, and the pressure may be normal.
It should be noted that the aging treatment and the drying treatment are different in preferable modes depending on the treatment time, the treatment temperature, and the degree of vacuum.

With respect to the above-described embodiment, the present invention further discloses the following coating particle group for monohalogenoamine production and a method for producing a coating particle group for monohalogenoamine production.

<1>
At least a part of the particles of the (A) solid ammonium salt (hereinafter referred to as the (A) component) is coated with the (C) water-soluble binder (hereinafter referred to as the (C) component), and further, the (A) component. A group of coated particles for producing monohalogenoamine, which comprises coated particles in which particles of a solid alkaline agent (hereinafter referred to as (B) component) are attached to the component (C) coated with.

<2>
Component (A), ammonium salts containing ammonium ion (NH 4 ^₊₎ (hereinafter referred to as inorganic ammonium salts) ammonium salt containing an organic ammonium ion (hereinafter, referred to as organic ammonium salts) a solid ammonium salt selected from, The coating particle group for producing monohalogenoamine according to <1> above, which is a solid ammonium salt preferably selected from inorganic ammonium salts.

<3>
The inorganic ammonium salts include ammonium chloride, ammonium sulfate, triammonium phosphate, ammonium dihydrogen phosphate, ammonium nitrate, ammonium bromide, ammonium iodide, ammonium carbonate, ammonium hydrogencarbonate, ammonium oxalate, ammonium acetate, ammonium lactate, and The coating particle group for producing monohalogenoamine according to <2> above, which is a solid ammonium salt selected from ammonium citrate.

<4>
The coating particle group for producing a monohalogenoamine according to <2>, wherein the organic ammonium salt is a solid ammonium salt selected from a primary ammonium salt and a secondary ammonium salt.

<5>
The component (A) is a compound selected from ammonium chloride, ammonium sulfate, triammonium phosphate, ammonium dihydrogen phosphate, ammonium nitrate, ammonium bromide, ammonium iodide, ammonium carbonate and ammonium hydrogen carbonate, preferably ammonium chloride. A compound selected from ammonium sulfate, triammonium phosphate, ammonium dihydrogen phosphate, ammonium nitrate, ammonium carbonate and ammonium hydrogen carbonate, more preferably ammonium chloride, still more preferably ammonium chloride, the above <1> to < The coating particle group for producing monohalogenoamine according to any one of 3>.

<6>
The pair ions of the component (A) are chloride ion, sulfate ion, phosphate ion, hydrogen phosphate ion, dihydrogen phosphate ion, nitrate ion, bromide ion, iodide ion, carbonate ion, hydrogen carbonate ion, and oxalic acid. A pair ion selected from an ion, an acetate ion, a lactate ion, and a citrate ion, preferably a chloride ion, a sulfate ion, a phosphate ion, a hydrogen phosphate ion, a dihydrogen phosphate ion, a nitrate ion, and a bromide ion. Pair ions selected from iodide ion, carbonate ion, and hydrogen carbonate ion, more preferably chloride ion, sulfate ion, phosphate ion, hydrogen phosphate ion, dihydrogen phosphate ion, nitrate ion, carbonate ion, The coating particle group for producing monohalogenoamine according to any one of <1> to <5> above, which is a counter ion selected from hydrogen carbonate ions, more preferably chloride ions.

<7>
The average particle size of the particles of the component (A) is 100 μm or more, preferably 300 μm or more, more preferably 500 μm or more, still more preferably 700 μm or more, still more preferably 800 μm or more, and 5,000 μm or less, preferably 3, The coating for monohalogenoamine production according to any one of <1> to <6> above, which is 000 μm or less, more preferably 2,000 μm or less, still more preferably 1,800 μm or less, still more preferably 1,500 μm or less. Particle swarm.

<8>
The component (B) is alkali metal hydroxide, alkaline earth metal hydroxide, alkali metal silicate, alkali metal oxide, alkaline earth metal oxide, alkali metal coal oxide, and alkaline earth metal coal oxide. The solid alkaline agent selected from, preferably a solid alkaline agent selected from alkaline earth metal hydroxides, more preferably calcium hydroxide, according to any one of <1> to <7> above. Coated particle group for monohalogenoamine production.

<9>
The coating particle group for producing monohalogenoamine according to <8>, wherein the alkali metal hydroxide is a compound selected from potassium hydroxide and sodium hydroxide, preferably potassium hydroxide.

<10>
The pre-alkali earth metal hydroxide is a compound selected from calcium hydroxide, magnesium hydroxide, magnesium hydroxide hydroxide, and calcium hydroxide, preferably a compound selected from calcium hydroxide and magnesium hydroxide. The coating particle group for producing monohalogenoamine according to <8>, which is more preferably calcium hydroxide.

<11>
The production of monohalogenoamine according to <8>, wherein the alkali metal silicate is a compound selected from sodium silicate and potassium silicate, preferably sodium silicate, and more preferably sodium metasilicate. Coating particle group for.

<12>
The coating particle group for producing monohalogenoamine according to <8>, wherein the alkali metal oxide is a compound selected from sodium oxide and potassium oxide.

<13>
The coating particle group for producing monohalogenoamine according to <8>, wherein the alkaline earth metal oxide is a compound selected from magnesium oxide and calcium oxide.

<14>
The coating particle group for producing monohalogenoamine according to <8>, wherein the alkali metal coal oxide is a compound selected from sodium carbonate and potassium carbonate, preferably sodium carbonate.

<15>
The coating particle group for producing monohalogenoamine according to <8>, wherein the alkaline earth metal coal oxide is a compound selected from calcium carbonate and magnesium carbonate, preferably calcium carbonate.

<16>
The coating for producing monohalogenoamine according to any one of <1> to <15>, wherein the average particle size of the particles of the component (B) is 5 μm or more, preferably 10 μm or more, 50 μm or less, preferably 30 μm or less. Particle swarm.

<17>
The component (C) is one or more selected from water-soluble polymer binders, preferably one or more selected from polyethylene glycol, polypropylene glycol, polyoxyethylene alkyl ether, and polyoxyethylene phenol ether. More preferably, it is one or more selected from polyethylene glycol, polypropylene glycol and polyoxyethylene alkyl ether, further preferably one or more selected from polyethylene glycol and polypropylene glycol, and even more preferably polyethylene glycol. The coating particle group for producing monohalogenoamine according to any one of <1> to <16>.

<18>
(C) The above-mentioned <1> to <17>, wherein the number average molecular weight of the component is 4,000 or more, preferably 6,000 or more, and 20,000 or less, preferably 13,000 or less. A group of coated particles for the production of monohalogenoamines.

<19>
Any of the above <1> to <18>, wherein the average particle size of the coating particle group for monohalogenoamine production is 100 μm or more, preferably 500 μm or more, and 5,000 μm or less, preferably 3,000 μm or less. The coated particle group for producing monohalogenoamines described.

<20>
The content of the component (A) in the coating particle group for producing monohalogenoamine is 30% by mass or more, preferably 40% by mass or more, more preferably 50% by mass or more, and 80% by mass or less, preferably 70% by mass. % Or less, more preferably 60% by mass or less, still more preferably 55% by mass or less, the coating particle group for producing monohalogenoamine according to any one of <1> to <19>.

<21>
The content of the component (B) in the coating particle group for monohalogenoamine production is 10% by mass or more, preferably 20% by mass or more, and 50% by mass or less, preferably 40% by mass or less. > To <20>. The coated particle group for producing monohalogenoamine.

<22>
The content of the component (C) in the coating particle group for monohalogenoamine production is 10% by mass or more, preferably 15% by mass or more, and 40% by mass or less, preferably 30% by mass or less, more preferably 20% by mass. % Or less, more preferably 18% by mass or less, according to any one of <1> to <21>.

<23>
The mass ratio (A) / (B) of the content of the component (A) to the content of the component (B) in the coating particle group for producing monohalogenoamine is 0.5 or more, preferably 1 or more, more preferably. The coating particle group for producing a monohalogenoamine according to any one of <1> to <22> above, which is 1.5 or more, and 3 or less, preferably 2.5 or less, more preferably 2 or less.

<24>
The mass ratio (A) / (C) of the content of the component (A) to the content of the component (C) in the coating particle group for producing monohalogenoamine is 0.5 or more, preferably 1 or more, more preferably. The coating particle for producing a monohalogenoamine according to any one of <1> to <23> above, which is 2 or more, more preferably 2.7 or more, and 6 or less, preferably 5 or less, more preferably 4 or less. group.

<25>
The total content of the components (A), (B) and (C) in the coating particle group for producing monohalogenoamine is 70% by mass or more, preferably 80% by mass or more, and 100% by mass or less, preferably 100% by mass or less. Is 90% by mass or less, the coating particle group for producing monohalogenoamine according to any one of <1> to <24>.

<26>
The product according to any one of <1> to <24> above, wherein the total content of the component (A), the component (B) and the component (C) is 100% by mass in the coating particle group for producing monohalogenoamine. Coated particle group for producing halogenoamine.

<27>
(D) Used for the production of monohalogenoamine by mixing in water with a compound that releases hypochlorous acid and / or hypochlorous acid ion when dissolved in water (hereinafter referred to as component (D)). The coating particle group for producing monohalogenoamine according to any one of <1> to <26>.

<28>
The production of monohalogenoamine according to <27> above, wherein the component (D) is a solid compound, preferably a solid compound that releases hypochlorous acid and / or hypochlorite ions when dissolved in water. Coating particle group for.

<29>
The components (D) are (D1) halogenated isocyanuric acid and its salt (hereinafter referred to as (D1) component), (D2) halogenated hydantine (hereinafter referred to as (D2) component) and (D3) hypohalite. The coating particle group for producing a monohalogenoamine according to <27>, which is a compound selected from (hereinafter, referred to as the component (D3)).

<30>
One or more of the components (D1) selected from sodium dichloroisocyanurate, potassium dichloroisocyanuric acid, trichloroisocyanuric acid, sodium bromoisocyanuric acid, potassium bromoisocyanuric acid, dibromoisocyanuric acid, tribromoisocyanuric acid, and triiodoisocyanuric acid. The coated particle group for producing monohalogenoamine according to <29>.

<31>
The component (D2) is selected from chlorodimethyl hydantoin, dichlorodimethyl hydantoin, bromodimethyl hydantoin, dibromodimethyl hydantoin, iododimethyl hydantoin, diiododimethyl hydantoin, bromochlorodimethyl hydantoin, chloroiododimethyl hydantoin, and bromoiododimethyl hydantoin 1 The coating particle group for producing monohalogenoamine according to <29>, which is more than one species.

<32>
(D3) Ingredients are from sodium hypochlorite, calcium hypochlorite, magnesium hypochlorite, calcium hypochlorite chloride, magnesium hypochlorite chloride, sodium hypochlorite, sodium hypoiodide. The coating particle group for producing monohalogenoamine according to <29>, which is one or more selected.

<33>
The component (D) is sodium dichloroisocyanurate, potassium dichloroisocyanuric acid, trichloroisocyanuric acid, chlorodimethylhydranthin, dichlorodimethylhydranthin, sodium hypochlorite, calcium hypochlorite, magnesium hypochlorite, hypochlorite chloride. A compound selected from calcium acid and magnesium hypochlorite, preferably a compound selected from sodium dichloroisocyanurate, trichloroisocyanuric acid, and calcium hypochlorite, more preferably calcium hypochlorite. A group of coated particles for producing monohalogenoamine according to <29>.

<34>
A method for producing a coated particle group for producing monohalogenoamine, which comprises the following steps (1) and (2).
Step (1): Particles of (A) solid ammonium salt (hereinafter referred to as (A) component) and (C) water-soluble binder (hereinafter referred to as (C) component) are mixed, and at least a part of the surface is covered. Step of obtaining a coated particle group (1) composed of particles of the component (A) coated with the component (C) Step (2): The coated particle group (1) and (B) solid alkali obtained in the step (1). The particles of the agent (hereinafter referred to as the component (B)) are mixed, and the particles of the component (B) are added to the component (C) coated with the component (A) of the coated particle group (1) obtained in the step (1). Step of obtaining a coated particle group (2) composed of particles to which

<35>
The monohalogenoamine production according to <34> above, wherein in the step (1), the component (C) is melted in part or all in advance and then mixed, preferably the component (C) is melted in advance and then mixed. A method for producing a coating particle group for use.

<36>
In the step (1), the mass ratio (A) / (C) of the content of the component (A) and the content of the component (C) in the coated particle group (1) is 0.5 or more, preferably 1 or more. The monohalogeno according to <34> or <35>, wherein the mixture is more preferably 2 or more, further preferably 2.7 or more, and 6 or less, preferably 5 or less, more preferably 4 or less. A method for producing a coated particle group for producing an amine.

<37>
The method for producing a coating particle group for monohalogenoamine production according to any one of <34> to <36>, wherein the component (C) is added to the component (A) and mixed in the step (1).

<38>
In the step (1), the rate of addition when the component (C) is melted and added in advance is 1,000 g / min or less, preferably 600 g / min or less, more preferably 200 g with respect to 100 g of the component (C). The method for producing a coating particle group for producing a monohalogenoamine according to <37>, wherein the content is less than / min, more preferably 150 g / min or less, still more preferably 100 g / min or less.

<39>
In step (1), the mixture is mixed using a granulator, and the Froude number of the granulator defined by the following formula is set to 50 or less, preferably 40 or less, more preferably 30 or less, still more preferably 20. Hereinafter, the method for producing a coating particle group for producing monohalogenoamine according to any one of <34> to <38>, which is more preferably 10 or less.
Froude number: Fr = V ² / (R × g)
V: Peripheral speed [m / s]
R: Radius from the center of rotation to the circumference of the rotating object [m]
g: Gravity acceleration [m / s ² ]
[In the formula, in a vertical or horizontal granulator equipped with a main wing and a crushing wing, V and R use the values of the main shaft, and in a Nauter mixer in which the stirring part draws a rotation and revolution trajectory, V and R rotate. The value of the stirring shaft will be used. ]

<40>
The above-mentioned <34> to <39>, wherein in the step (1), the temperature at the time of mixing is 60 ° C. or higher, preferably 70 ° C. or higher, and 100 ° C. or lower, preferably 90 ° C. or lower. A method for producing a coated particle group for producing monohalogenoamine.

<41>
In the step (2), the mass ratio (A) / (B) of the content of the component (A) and the content of the component (B) in the coated particle group (2) is 0.5 or more, preferably 1 or more. The monohalogenoamine according to any one of <34> to <40>, which is mixed so as to be more preferably 1.5 or more, and 3 or less, preferably 2.5 or less, more preferably 2 or less. A method for producing a coating particle group for production.

<42>
In the step (2), the mixture is mixed using a granulator, and the Froude number of the granulator defined by the above formula is set to 50 or less, preferably 40 or less, more preferably 30 or less, still more preferably 20 or less. The method for producing a coated particle group for producing monohalogenoamine according to any one of <34> to <41>, wherein the content is even more preferably 10 or less.

<43>
The above-mentioned <34> to <42>, wherein in the step (2), the temperature at the time of mixing is 60 ° C. or higher, preferably 70 ° C. or higher, and 100 ° C. or lower, preferably 90 ° C. or lower. A method for producing a coated particle group for producing monohalogenoamine.

<44>
The method for producing a coated particle group for producing a monohalogenoamine according to any one of <34> to <43>, further comprising the following step (3).
Step (3): A step of drying the coated particle group (2) obtained in the step (2).

<45>
In step (3), the drying time is 1 hour or more, preferably 2 hours or more, more preferably 5 hours or more, preferably 8 hours or more, and 24 hours or less, preferably 16 hours or less. > To <44>. The method for producing a coating particle group for producing monohalogenoamine.

<46>
In the step (3), the drying temperature is 10 ° C. or higher, preferably 20 ° C. or higher, more preferably 25 ° C. or higher, and 70 ° C. or lower, preferably 60 ° C. or lower, more preferably 55 ° C. or lower. 34> The method for producing a coating particle group for producing a monohalogenoamine according to any one of <45>.

<47>
In the step (3), the drying treatment is vacuum drying, and the degree of vacuum is 10 kPa abs or more, preferably 15 kPa abs or more, and 50 kPa abs or less, preferably 40 kPa abs or less. The method for producing a coating particle group for producing monohalogenoamine according to any one of.

The reagents used in Examples and Comparative Examples are as follows.
(A) Ingredients-Ammonium chloride: Zhuzhou JianhgHai EnvironmentProtectionCo. Ltd, average particle size 1 mm
(B) Ingredients-Calcium hydroxide: manufactured by Tomita Pharmaceutical Co., Ltd., average particle size 20 μm
(C) Ingredients-PEG: Polyethylene glycol, manufactured by Kao Corporation, K-PEG6000LA, number average molecular weight 8,500

The average particle size of the component (A) and the coated particle group of the present invention is 2,000, 1, After vibrating for 5 minutes using a sieve of 400, 1,000, 710, 500, 355, 250, 180, 125, 90, 63, 45 μm, the 50% average diameter is calculated for the mass distribution under the sieve by the sieving method. Then, this was taken as the average particle size. Specifically, JISZ8801-1 (established on May 20, 2000, final revision on November 20, 2006) 2,000, 1,400, 1,000, 710, 500, 355, 250, 180, Using a 125, 90, 63, 45 μm sieve, stack the sieves on the saucer in order from the smallest mesh, add 100 g of the particles from the top 2,000 μm sieve, cover and low-tap sieve. Attached to a shaker (manufactured by HEIKO Seisakusho, tapping 156 times / minute, rolling: 290 times / minute), vibrated for 5 minutes, then measured the mass of the particles remaining on each sieve and saucer, and each sieve. The mass ratio (%) of the above particles was calculated. The mass ratios of the particles on a sieve having a small opening were integrated in order from the saucer, and the particle size at which the total was 50% was defined as the average particle size.

The average particle size of the component (B) is a value measured under the following conditions using a laser diffraction / scattering type particle size distribution measuring device (LA-920 manufactured by HORIBA).
Solvent: Ethanol Refractive index: 1.2
Circulation speed: 4
Circulation: 3min

The number average molecular weight of the component (C) is a value measured by a gel permeation chromatography (GPC) method using polystyrene as a standard using water / ethanol as a solvent.

Example 1
157.5 g of ammonium chloride was put into a high speed mixer (manufactured by Fukae Powtech Co., Ltd., capacity 2 L), and 52.5 g of PEG previously melted to a temperature equal to or higher than the melting point was added to 50 g / while stirring under the conditions shown in Table 1. It was added at a rate of 1 minute and mixed for 1 minute to obtain a coated particle group (1) composed of the component (A) in which at least a part of the surface was coated with the component (C) (step (1)). Then, 90 g of calcium hydroxide was added to the obtained coated particle group (1) and mixed for 1 minute under the conditions shown in Table 1 to coat the component (A) of the coated particle group (1) (C). A coated particle group (2) composed of particles to which the component (B) was attached to the component () was obtained (step (2)). The average particle size of the coated particle group (2) was 1,157 μm.

Further, with respect to the coated particle group of Example 1, by observing the surface of the component (A) and the surface of the coated particle group (2) with an electron microscope (SEM), the coated particle group (2) becomes the component (A). It was confirmed that the particle structure was such that the component (B) was attached to the component (C) coated with. A photograph of the surface structure of the component (A) is shown in FIG. 1, and a photograph of the surface structure of the coated particle group (2) is shown in FIG.

Example 2
After producing the coated particle group (2) under the same conditions as in Example 1, the coated particle group (2) was stored in a desiccator and dried at a vacuum degree of 20 kPa abs and a drying temperature of 25 ° C. for 12 hours. The average particle size of the coated particle group (2) was 1,160 μm.

Example 3
After producing the coated particle group (2) under the same conditions as in Example 1, the coated particle group (2) was placed in a PP bottle, sealed and aged at room temperature for 6 days, and then the coated particle group (2) was stored in a desiccator and dried at a vacuum degree of 20 kPa abs. The drying treatment was carried out at a temperature of 25 ° C. for 12 hours. The average particle size of the coated particle group (2) was 1,212 μm.

Example 4
The coated particle group (2) was produced under the same conditions as in Example 1 except that the jacket temperature of the high-speed mixer was set to 40 ° C. The average particle size of the coated particle group (2) was 1,057 μm.

Example 5
After producing the coated particle group (2) under the same conditions as in Example 1, the coated particle group (2) is stored in an electric dryer (ADVANTEC, DRM620TA) and dried on a shelf at 50 ° C. for 2 hours in an open state. Processing was performed. The average particle size of the coated particle group (2) was 1,175 μm.

Example 6
After producing the coated particle group (2) under the same conditions as in Example 1, the coated particle group (2) was put into a fluidized bed (SPIR-A-FLOW manufactured by FREUND) at 50 ° C. and an air volume of 3.5 m ³ The drying treatment was performed at / min for 0.5 hours. The average particle size of the coated particle group (2) was 1,166 μm.

Example 7
The coated particle group (2) was produced under the same conditions as in Example 2 except that ammonium chloride was 171.9 g, PEG was 30.3 g, and calcium hydroxide was 97.8 g. The average particle size of the coated particle group (2) was 912 μm.

Example 8
The coated particle group (2) was produced under the same conditions as in Example 2 except that ammonium chloride was 153.9 g, PEG was 58.2 g, and calcium hydroxide was 87.9 g. The average particle size of the coated particle group (2) was 1,276 μm.

Comparative Example 1
63.6 g of ammonium chloride and 36.4 g of calcium hydroxide were stirred in a beaker using a spatula to obtain a mixture.

[Evaluation of dissolution time]
500 g of ion-exchanged water was placed in a 1 L beaker, and the amount of the coated particle group of the example and the mixture of the comparative example were adjusted so that the amount of ammonium chloride as the component (A) was 1.75 g. .. The 1 L beaker was shaken by hand to dissolve the granulated product, and the time until the particles could not be visually confirmed was defined as the dissolution time. The results are shown in Table 1. If the dissolution time is within 3 minutes, it can be said that the solubility is good.

[(D) Evaluation of heat generation suppression when contacting components]
As a component (D), 2.25 g of calcium hypochlorite (Toyocron-PTGIII of Toso Co., Ltd., effective chlorine 70.5%, particle size 2-5 mm) and 3.34 g of a mixture of the coated particle group of Examples and Comparative Examples were used. Put them in 100cc polypropylene cups (upper diameter x lower diameter x height: φ60 x φ44 x 74mm), stir with a glass rod for 50 rotations per minute so that the entire sample is mixed, and then use a glass thermometer (Nippon Keiki). The reading of the thermometer reading 1 minute after the start of stirring was read with an ISO-compatible rod-shaped thermometer manufactured by Kogyo Co., Ltd., and the heat generation suppression effect was evaluated according to the following criteria. The results are shown in Table 1.
A: Temperature rise is less than 3 ° C B: Temperature rise is 3 ° C or more and less than 5 ° C C: Temperature rise is 5 ° C or more and less than 10 ° C D: Temperature rise is 10 ° C or more

[Ammonia odor evaluation of agent]
5 g of each of the coated particle group of the example and the mixture of the comparative example were put into a 200 cc polypropylene cup (upper diameter x lower diameter x height: φ83 x φ58 x 85 mm), and 5 panelists sniffed the odor according to the following criteria. The strength of the odor was evaluated in consultation with five panelists. The results are shown in Table 1.
A: Smell faintly B: Smell a little C: Smell D: Very strong odor, dangerous to smell

In addition, 5 g of each of the coated particle group of Example and the mixture of Comparative Example were placed in a vial with an inner plug (Vacuum Vial White SVF-100 of Nichiden Rika Glass Co., Ltd.), sealed and stored at 50 ° C. for 1 week. .. The strength of the ammonia odor after storage was evaluated by the same method as described above. The results are shown in Table 1.

[Evaluation of monochrome lamin production]
It was confirmed that monochlorolamin was produced by mixing the coated particle group of the example and the mixture of the comparative example with the aqueous sodium hypochlorite solution, respectively.

By combining the solid ammonium salt and the solid alkaline agent into one agent in comparison with the examples of the present invention and the comparative example, monohalogenoamine can be easily synthesized in combination with a halogen agent, and the dissolution rate in water is also good. It turns out that. It can also be seen that the heat generation at the time of contact with the solid halogen agent is suppressed, and the ammonia odor of the agent is also suppressed.

Claims (7)

At least a part of the particles of the (A) solid ammonium salt (hereinafter referred to as the (A) component) is coated with the (C) water-soluble binder (hereinafter referred to as the (C) component), and further, the (A) component. A group of coated particles for producing monohalogenoamine, which comprises coated particles in which particles of a solid alkaline agent (hereinafter referred to as (B) component) are attached to the component (C) coated with. The coating particle group for monohalogenoamine production according to claim 1, wherein the mass ratio (A) / (B) of the content of the component (A) to the content of the component (B) is 0.5 or more and 3 or less. .. The coating for producing a monohalogenoamine according to claim 1 or 2, wherein the mass ratio (A) / (C) of the content of the component (A) to the content of the component (C) is 0.5 or more and 6 or less. Particle swarm. A method for producing a coated particle group for producing monohalogenoamine, which comprises the following steps (1) and (2).
Step (1): Particles of (A) solid ammonium salt (hereinafter referred to as (A) component) and (C) water-soluble binder (hereinafter referred to as (C) component) are mixed, and at least a part of the surface is covered. Step of obtaining a coated particle group (1) composed of particles of the component (A) coated with the component (C) Step (2): The coated particle group (1) and (B) solid alkali obtained in the step (1). The particles of the agent (hereinafter referred to as the component (B)) are mixed, and the particles of the component (B) are added to the component (C) coated with the component (A) of the coated particle group (1) obtained in the step (1). Step of obtaining a coated particle group (2) composed of particles to which The method for producing a coated particle group for producing a monohalogenoamine according to claim 4, further comprising the following step (3).
Step (3): A step of drying the coated particle group (2) obtained in the step (2). In the step (1), the mass ratio (A) / (C) of the content of the component (A) and the content of the component (C) in the coated particle group (1) is 0.5 or more and 6 or less. The method for producing a coating particle group for producing a monohalogenoamine according to claim 4 or 5, which is mixed with. In the step (2), the mass ratio (A) / (B) of the content of the component (A) and the content of the component (B) in the coated particle group (2) is 0.5 or more and 3 or less. The method for producing a coating particle group for producing a monohalogenoamine according to any one of claims 4 to 6, which is mixed with.

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