JP2018087123A - Coating particles for manufacturing mono-halogen amine - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide coating particles for manufacturing mono-halogen amine capable of simply synthesizing mono-halogen amine with combination with a halogen agent by unifying a solid ammonium salt and a solid alkaline agent, good in dissolution rate to water and suppressing ammonia odor of the agent, and a manufacturing method of the coating particles for manufacturing mono-halogen amine.SOLUTION: There are provided coating particles for manufacturing mono-halogen amine in which at least a part of particles of a solid ammonium salt (hereafter (A) component), is coated with (C) a water soluble binder (hereafter (C) component), and particles of (B) a solid alkali agent (hereafter (B) component) adhere to the (C) component coating the (A) component.SELECTED DRAWING: None

Description

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

Chlorine-containing compounds are sterilizing treatments in a wide range of fields such as foods, medical instruments, kitchen utensils, daily utensils, indoor cleaning sterilization, sterilization of human bodies and animals, plants, tubs and pools, and sterilization. Has been used.
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 with organic substances, and the bactericidal effect is lowered due to the alkaline pH. Therefore, we focused on monochloramine, a kind of bound chlorine, as a disinfectant to replace hypochlorous acid.
Monochloramine has advantages in that it does not easily react with organic substances compared to hypochlorous acid and has a long-lasting effect, hardly corrodes metal materials, has high persistence, and acts on biofilms. On the other hand, since the storage stability at a high concentration is poor, it is generally used by so-called preparation at the time of use, which is generated each time it is used.
Monochloramine is obtained by reacting chlorine or hypochlorous acid with ammonia.

  In Patent Document 1, in a method of synthesizing monochloramine by a reaction between an ammonium chloride solution and a sodium hypochlorite solution, the sodium hypochlorite solution is made alkaline with an inorganic base in advance, and the reaction medium contains A method is described in which the ratio of the concentration of ammonium chloride to the concentration of sodium hypochlorite in the reaction medium is 1 to 1.5.

  In the example of Patent Document 2, a protozoan of a circulating water purification tank that synthesizes monochloramine by injecting ammonia water or ammonium salt water and sodium hypochlorite solution directly into a source tank using a drug pump. An inactivation method is disclosed.

JP 20041555651 A JP 2008-264678 A

In Patent Document 1 and Patent Document 2, monochloramine is generated from a liquid raw material, and in order to prepare and use it as a disinfectant or disinfectant, a large amount of raw material storage space and complicated operations must be accepted. .
When monohalogenamine such as monochloramine is generated, a compound that releases hypohalous acid and / or hypohalous acid 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 monohalogenoamines, but adding three kinds individually requires complicated operations from the user's side and is easy to use. Is bad. In addition, when the three types are mixed to form a single agent, the halogen agent and the solid ammonium salt generate rapid heat generation due to oxidation / reduction reactions, and thus both must be formulated separately. On the other hand, when a solid ammonium salt and a solid alkali agent are mixed to form a single agent, ammonia is generated due to a neutralization reaction, which is a problem.

  In the present invention, by combining a solid ammonium salt and a solid alkali agent into one agent, a 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 is reduced. Provided are a method for producing a coated particle group for producing monohalogenoamine and a coated particle group for producing monohalogenoamine.

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

Moreover, this invention relates to the manufacturing method of the coated particle group for monohalogenoamine manufacture which has the following process (1) and (2).
Step (1): (A) Solid ammonium salt (hereinafter also referred to as component (A)) particles and (C) a water-soluble binder (hereinafter also referred to as component (C)) are mixed, and at least one surface is mixed. Step of obtaining a coated particle group (1) composed of particles of component (A) coated with component (C) part Step (2): Coated particle group (1) and (B) obtained in step (1) The component (C) in which the component (A) of the coated particle group (1) obtained in the step (1) is mixed with the component (B) is mixed with particles of a solid alkaline agent (hereinafter also referred to as the component (B)). Step of obtaining a coated particle group (2) composed of particles to which component particles are attached

  According to the present invention, by combining a solid ammonium salt and a solid alkali agent into a single agent, a 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 method for producing a coated particle group for producing a monohalogenoamine and a coated particle group for producing a monohalogenoamine for suppressing odor.

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

<Coated particles 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) (B) ) A coated particle group consisting of coated particles to which component particles are attached.

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

  Inorganic ammonium salts include ammonium chloride, ammonium sulfate, triammonium phosphate, ammonium dihydrogen phosphate, ammonium nitrate, ammonium bromide, ammonium iodide, ammonium carbonate, ammonium bicarbonate, ammonium oxalate, ammonium acetate, ammonium lactate, citric acid. An ammonium acid is mentioned.

  Examples of organic ammonium salts include primary ammonium salts and secondary ammonium salts. Here, the primary ammonium salt is one in which one of the hydrogen atoms of the ammonium ion is substituted with a group containing carbon, and the secondary ammonium salt is one in which two of the hydrogen atoms of the 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 monohalogenamine 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 monohalogenamine production rate. .
The component (A) is more preferably ammonium chloride from the viewpoint of increasing the monohalogenamine production rate.

The counter ion of component (A) is preferably chloride ion, sulfate ion, phosphate ion, hydrogen phosphate ion, diphosphate phosphate from the viewpoint of suppressing the decomposition of monohalogenamine and increasing the production rate of monohalogenamine. It is selected from hydrogen ion, nitrate ion, bromide ion, iodide ion, carbonate ion, bicarbonate 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, phosphate from the viewpoint of suppressing the decomposition of monohalogenamine and increasing the production rate of monohalogenamine. It is selected from dihydrogen ions, nitrate ions, bromide ions, iodide ions, carbonate ions, and bicarbonate ions.
The counter ion of component (A) is more preferably chloride ion, sulfate ion, phosphate ion, hydrogen phosphate ion, phosphate from the viewpoint of suppressing the decomposition of monohalogenamine and increasing the production rate of monohalogenamine. It is selected from dihydrogen ions, nitrate ions, carbonate ions, and bicarbonate ions.
The counter ion of the component (A) is more preferably a chloride ion from the viewpoint of suppressing the decomposition of the monohalogenamine and increasing the production rate of the monohalogenamine. The component (A) is more preferably an ammonium salt composed of ammonium ions and chloride ions, that is, ammonium chloride.

  The average particle size of the component (A) particles 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, and still more preferably 800 μm, from the viewpoints of handling properties and solubility. Above, and preferably 5,000 μm or less, more preferably 3,000 μm or less, still more preferably 2,000 μm or less, even more preferably 1,800 μm or less, and even more preferably 1,500 μm or less. An average particle diameter can be measured by using the method as described in an Example.

[Component (B)]
(B) A component is a solid alkali agent. The component (B) becomes a monohalogenamine decomposition inhibitor during monohalogenamine synthesis. 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 carbonate, and an alkaline earth metal carbonate. It is a solid alkali agent selected from.

The alkali metal hydroxide of component (B) includes potassium hydroxide and sodium hydroxide from the viewpoint of suppressing the decomposition of monohalogenamine and increasing the production rate of monohalogenamine, and potassium hydroxide is preferred.
The alkaline earth metal hydroxide of component (B) includes calcium hydroxide and magnesium hydroxide from the viewpoint of suppressing the decomposition of monohalogenamine and increasing the production rate of monohalogenamine, and calcium hydroxide is preferred. Examples of the alkaline earth metal hydroxide include alkaline earth metal chloride hydroxides such as magnesium chloride hydroxide and calcium chloride hydroxide.
Examples of the alkali metal silicate (B) include sodium silicate and potassium silicate from the viewpoint of suppressing the decomposition of monohalogenamine and increasing the production rate of monohalogenamine, and sodium silicate is preferred. The sodium silicate is preferably sodium metasilicate.
Alkali metal oxides and alkaline earth metal oxides react with water to become alkali metal hydroxides or alkaline earth metal hydroxides, and therefore 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.
The alkali metal carbonate as the component (B) includes sodium carbonate and potassium carbonate from the viewpoint of suppressing the decomposition of monohalogenamine and increasing the production rate of monohalogenamine, and sodium carbonate is preferable.
The alkaline earth metal carbonate of component (B) includes calcium carbonate and magnesium carbonate from the viewpoint of suppressing the decomposition of monohalogenamine and increasing the production rate of monohalogenamine, and calcium carbonate is preferred.
The component (B) is preferably an alkaline earth metal hydroxide and more preferably calcium hydroxide from the viewpoint of suppressing the decomposition of the monohalogenamine and increasing the production rate of the monohalogenamine.

  The average particle size of the component (B) particles 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 the coverage and solubility in the component (A). It is. The average particle diameter can be measured by using a laser diffraction / scattering particle size distribution measuring apparatus (for example, LA-920, manufactured by HORIBA).

[Component (C)]
Component (C) is a water-soluble binder. The component (C) is to coat at least a part of the particles of the component (A) with the component (C), thereby reducing direct contact between the particles of the component (B) and the component (A) to be subsequently adhered. Thus, 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 viewpoints of solubility in water and coverage.
Specific examples of the component (C) include polyethylene glycol, polypropylene glycol, polyoxyethylene alkyl ether, polyoxyethylene phenol ether and the like from the viewpoints of solubility in water and covering properties. One or more selected from polyoxyethylene alkyl ethers are preferred, one or more selected from polyethylene glycol and polypropylene glycol are more preferred, and polyethylene glycol is even more preferred.

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. It 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. 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 a monohalogenoamine according to the present invention is a coated particle group for producing a monohalogenoamine comprising particles containing the component (A), the component (B), and the component (C), and the component (A) At least a part of the particles is coated with the component (C), and further, an aggregate of particles having a structure in which the particles of the component (B) are attached to the component (C) coated with the component (A).
That is, the coated particle group for producing monohalogenoamine of the present invention comprises (A) component particles, (C) component first coating layer that coats the surface of component (A) particles, and first coating layer. It is the aggregate | assembly of the particle | grains which have the 2nd coating layer which consists of (B) component formed on the top.
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) (B) ) Contains coated particles to which component particles 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 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 coated 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 viewpoints of handling properties and solubility. 000 μm or less. An average particle diameter can be measured by using the method as described in an Example.

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

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

  The content of the component (C) in the monohalogenoamine-coated coated particle group of the present invention is preferably 10% by mass or more from the viewpoints of storage stability, coatability to the component (B), and suppression of ammonia odor. Preferably it is 15 mass% or more, and preferably 40 mass% or less, More preferably, it is 30 mass% or less, More preferably, it is 20 mass% or less, More preferably, it is 18 mass% or less. The content of the component (C) in the monohalogenoamine-coated coated particle group can be determined by the amount charged at the time of manufacture, but can also be determined by a conventional method such as liquid chromatography.

  In the coated particle group for producing monohalogenoamine according to the present invention, the mass ratio (A) / (B) of the content of the component (A) and the content of the component (B) depends on the production rate and handling property of the monohalogenamine. 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 coated particle group for producing monohalogenoamine of the present invention, the mass ratio (A) / (C) of the content of the component (A) and the content of the component (C) depends on the storage stability and the component (B). From the viewpoint of covering properties and ammonia odor suppression, preferably 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. More preferably, it is 4 or less.

  The total content of the component (A), the component (B), and the component (C) in the coated particle group for producing the monohalogenoamine of the present invention is preferably from the viewpoint of monohalogenamine production rate, cost, and handling properties. 70% by mass or more, more preferably 80% by mass or more, and 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 comprises (D) a compound that releases hypohalous acid and / or hypohalite ion (hereinafter referred to as (D) component) and water when dissolved in water. Monohalogenamine can be synthesized by mixing.
Examples of the component (D) include compounds selected from (D1) halogenated isocyanuric acid and salts thereof, (D2) halogenated hydantoins, and (D3) hypohalites.
When the (D) component is a solid compound, the coated particle group for producing a monohalogenoamine of the present invention can suppress heat generation when the particle group and the (D) component of the solid compound are in contact with each other. From the viewpoint of sex.

(D1) Halogenated isocyanuric acid and salts thereof include, as specific examples, dichloroisocyanurates such as sodium dichloroisocyanurate and potassium dichloroisocyanurate, bromoisocyanurates such as trichloroisocyanuric acid, sodium bromoisocyanurate and potassium bromoisocyanurate. Examples thereof include acid salts, dibromoisocyanuric acid, tribromoisocyanuric acid, and triiodoisocyanuric acid.
(D2) Specific examples of halogenated hydantoins include chlorodimethylhydantoin, dichlorodimethylhydantoin, bromodimethylhydantoin, dibromodimethylhydantoin, iododimethylhydantoin, diiododimethylhydantoin, bromochlorodimethylhydantoin, chloroiododimethylhydantoin, and bromoiodo. Examples include dimethylhydantoin.
(D3) Specific examples of hypohalites include hypochlorous acid such as sodium hypochlorite, calcium hypochlorite, magnesium hypochlorite, calcium chloride hypochlorite, magnesium chloride hypochlorite and the like. Examples include chlorite, hypobromite such as sodium hypobromite, and hypoiodite such as sodium hypoiodite.

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.
The component (D) is preferably sodium dichloroisocyanurate, potassium dichloroisocyanurate, trichloroisocyanuric acid, chlorodimethylhydantoin, dichlorodimethylhydantoin, sodium hypochlorite, hypochlorous acid, from the viewpoint of increasing the production rate of monohalogenamine. It is a compound selected from calcium chlorate, magnesium hypochlorite, calcium chloride hypochlorite, and magnesium chloride 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 monohalogenamine.
The component (D) is more preferably calcium hypochlorite from the viewpoint of increasing the production rate of monohalogenamine.

Even if it is components other than (A)-(C) component, the coated particle group for monohalogenoamine manufacture of this invention can contain another component suitably in the range which can solve the subject of this invention. As other components, you may contain a fragrance | flavor, a pigment | dye, an antifoamer, a bulking agent, or a diluent. These components may be contained in the coated particles.
Examples of the extender or diluent include sulfates such as sodium sulfate and magnesium sulfate. If a bulking agent or a diluent is blended, each component can be diluted and dispersed at an appropriate concentration so that it can be designed in an amount suitable for use.

<Method for Producing Coated Particles for Monohalogenamine Production>
The method for producing a coated particle group for producing a monohalogenoamine according to the present invention is a method for producing a coated particle group for producing a monohalogenoamine having the following steps (1) and (2).
Step (1): Particles of component (A) and component (C) are mixed, and a coated particle group (1) comprising particles of component (A) whose surface is at least partially coated with component (C). Step (2): The coated particle group (1) obtained in the step (1) and the particles of the component (B) are mixed, and the (A) of the coated particle group (1) obtained in the step (1) is obtained. Step of obtaining coated particle group (2) comprising particles in which component (B) particles are attached to component (C) coated with component) The method for producing a coated particle group for producing monohalogenoamine according to the present invention is a monohalogenoamine. The matters described in the coated particle group for production can be appropriately applied.

[Step (1)]
In the 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) in which at least a part of the surface is coated with the component (C). It is a process.

  The component (C) may be partially or wholly melted in advance, or may be blended as a solid and heated and melted inside the mixer, but is preferably melted in advance.

  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) in the coated particle group (1) and the component (C) The mass ratio of the content of (A) / (C) is preferably from the viewpoints of uniformly suppressing the heat generation when the surface of the component (A) is uniformly coated and brought into contact with the white powder, and from the viewpoint of ammonia odor suppression 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. To do.

  In the step (1), from the viewpoint of the coverage of the component (A) with the component (C), a method of adding the component (C) to the component (A) is preferable. The addition rate when the component (C) is melted and added in advance is preferably 1,000 g / min or less, more preferably 100 g per 100 g of the component (C), from the viewpoint of improving 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, and still more preferably 100 g / min or less.

  When mixing each component in step (1), Henschel mixer (made by Mitsui Mining Co., Ltd.), high speed mixer (made by Fukae Powtech Co., Ltd.), Nauter mixer (made by Hosokawa Micron Co., Ltd.), ribbon Known mixers such as a type mixer (manufactured by Tokuju Co., Ltd.), a V-type blender (manufactured by Dalton Co., Ltd.), and a bench kneader (manufactured by Irie Shokai Co., Ltd.) can be used. The mixer is preferably a high speed mixer or a Henschel mixer from the viewpoint of the coverage of the component (C) to the component (A).

  From the viewpoint of suppressing coarsening and mixing of raw materials during mixing, the setting of the fluid number of the granulator defined by the following formula is preferably 50 or less, more preferably 40 or less, It is more preferably 30 or less, even more preferably 20 or less, and even more preferably 10 or less.

Fluid number: Fr = V ² / (R × g)
V: Circumferential 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 vertical or horizontal granulators equipped with main wings and crushing wings, V and R use the values of the main shaft, and in a Nauter mixer where the agitator draws a rotation and revolution orbit, V and R are rotation agitation shafts. The value of is used.

  In the step (1), the temperature during mixing (jacket temperature of the mixer) is preferably 60 from the viewpoint of suppressing the coagulation 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 (A) of the coated particle group (1) obtained in the step (1). This is a step of obtaining a coated particle group (2) composed of particles in which the component (B) is adhered to the component (C) coated with the component.

  In step (2), when the coated particle group (1) obtained in step (1) and the particles of component (B) are mixed to obtain the coated particle group (2), From the viewpoint of the heat generation suppression when the mass ratio (A) / (B) of the content of the component (A) and the content of the component (B) is in contact with the production rate of monohalogenamine, storage stability, and the powdered saliva. , 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).
In the step (2), the temperature during mixing (jacket temperature of the mixer) is preferably 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 coarsening during mixing and pulverization of the raw material, the setting of the fluid number of the granulator defined by the above formula is preferably 50 or less, and 40 or less. More preferably, it is more preferably 30 or less, even more preferably 20 or less, and even more preferably 10 or less.

[Step (3)]
The method for producing a coated particle group for producing monohalogenoamine of the present invention preferably further includes the following step (3) after step (2) from the viewpoint of reducing ammonia odor.
Step (3): 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 prevention. More preferably, it is 55 ° C. or lower.

In the step (3), the drying treatment can be selected from atmospheric shelf drying. In this case, the drying time is preferably 1 hour or longer, more preferably 2 hours or longer, and preferably 24 hours or shorter, more preferably 16 hours or shorter. 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, and further preferably 55 ° C. from the viewpoint of blocking inhibition. It is as follows.

In the step (3), the drying treatment can be selected from drying using a fluidized bed dryer. Examples of the fluidized bed dryer include SPIR-A-FLOW manufactured by FREUND. When performing the step (3) using a fluidized bed dryer, 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 from the viewpoint of blocking inhibition. More preferably, it is 60 degrees C or less, More preferably, it is 55 degrees C or less.
Moreover, from the viewpoint of drying efficiency, the blowing rate 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 longer, more preferably 0.4 hours or longer, and preferably 2 hours or shorter, more preferably 1 hour or shorter.

In the method for producing a coated particle group for producing 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 performing an aging treatment. The aging treatment period is not particularly limited, but is preferably within 1 month, more preferably within 2 weeks, most preferably within 1 week, and preferably 2 days or more, more preferably 3 from the viewpoint of productivity. 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 preferably sealed from the viewpoint of suppressing moisture absorption, and may be normal pressure.
Note that the aging treatment and the drying treatment differ in preferable modes depending on the treatment time, treatment temperature, and degree of vacuum.

  In relation to the above-described embodiment, the present invention further discloses the following method for producing monohalogenamine-coated coated particles and monohalogenamine-coated coated particles.

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

<2>
The component (A) is a solid ammonium salt selected from ammonium salts containing ammonium ions (NH ₄ ⁺ ) (hereinafter referred to as inorganic ammonium salts) and ammonium salts containing organic ammonium ions (hereinafter referred to as organic ammonium salts). The coated particle group for producing monohalogenoamine according to the above <1>, which is preferably a solid ammonium salt selected from inorganic ammonium salts.

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

<4>
The coated particle group for producing 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>
(A) component 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, <1> to <<1>, which is a compound selected from ammonium sulfate, triammonium phosphate, ammonium dihydrogen phosphate, ammonium nitrate, ammonium carbonate, and ammonium hydrogen carbonate, more preferably ammonium chloride, and even more preferably ammonium chloride. 3> The coated particle group for producing a monohalogenoamine according to any one of 3).

<6>
(A) Counter ion of component is chloride ion, sulfate ion, phosphate ion, hydrogen phosphate ion, dihydrogen phosphate ion, nitrate ion, bromide ion, iodide ion, carbonate ion, bicarbonate ion, oxalic acid A counter ion selected from ions, acetate ions, lactate ions, and citrate ions, preferably chloride ions, sulfate ions, phosphate ions, hydrogen phosphate ions, dihydrogen phosphate ions, nitrate ions, bromide ions, It is a counter ion 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, And any one of the above <1> to <5>, which is a counter ion selected from hydrogen carbonate ions, and more preferably a chloride ion. Mono-halogeno-amine producing coated particles according to.

<7>
The average particle size of the component (A) particles 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 producing monohalogenoamine according to any one of <1> to <6>, which is 000 μm or less, more preferably 2,000 μm or less, further preferably 1,800 μm or less, and still more preferably 1,500 μm or less. Particle group.

<8>
Component (B) is an alkali metal hydroxide, alkaline earth metal hydroxide, alkali metal silicate, alkali metal oxide, alkaline earth metal oxide, alkali metal carbonate, or alkaline earth metal carbonate <1> to <7>, which is a solid alkaline agent selected from: preferably a solid alkaline agent selected from alkaline earth metal hydroxides, more preferably calcium hydroxide. A group of coated particles for producing monohalogenoamines.

<9>
The coated 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-alkaline earth metal hydroxide is a compound selected from calcium hydroxide, magnesium hydroxide, magnesium chloride hydroxide, and calcium chloride hydroxide, preferably a compound selected from calcium hydroxide and magnesium hydroxide The coated particle group for producing monohalogenoamine according to <8>, more preferably calcium hydroxide.

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

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

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

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

<17>
Component (C) is at least one selected from water-soluble polymer binders, preferably at least one selected from polyethylene glycol, polypropylene glycol, polyoxyethylene alkyl ether, and polyoxyethylene phenol ether. More preferably, it is at least one selected from polyethylene glycol, polypropylene glycol and polyoxyethylene alkyl ether, still more preferably at least one selected from polyethylene glycol and polypropylene glycol, still more preferably polyethylene glycol, The coated particle group for producing a monohalogenoamine according to any one of <1> to <16>.

<18>
The number average molecular weight of the component (C) is 4,000 or more, preferably 6,000 or more, and 20,000 or less, preferably 13,000 or less, according to any one of <1> to <17> above Of coated particles for producing monohalogenoamines.

<19>
The average particle size of the coated particle group for producing monohalogenoamine is 100 μm or more, preferably 500 μm or more, and 5,000 μm or less, preferably 3,000 μm or less, in any one of the above items <1> to <18> The coated particle group for producing the monohalogenoamine as described.

<20>
The content of the component (A) in the coated 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, and still more preferably 55% by mass or less, the coated particle group for producing monohalogenoamine according to any one of <1> to <19>.

<21>
The content of the component (B) in the monohalogenoamine-coated coated particle group is 10% by mass or more, preferably 20% by mass or more, and 50% by mass or less, preferably 40% by mass or less, <1 The coated particle group for producing a monohalogenoamine according to any one of> to <20>.

<22>
The content of the component (C) in the monohalogenoamine-coated coated particle group 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, the coated particle group for producing monohalogenoamine according to any one of <1> to <21>.

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

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

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

<26>
Mono in any one of said <1>-<24> whose total content of (A) component, (B) component, and (C) component is 100 mass% in the covering particle group for monohalogenamine manufacture. Coated particle group for producing halogenoamine.

<27>
(D) mixed in water together with a compound that releases hypohalous acid and / or hypohalous acid ions (hereinafter referred to as component (D)) when dissolved in water, and used for monohalogenamine production, The coated particle group for producing a monohalogenoamine according to any one of <1> to <26>.

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

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

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

<31>
(D2) The component is selected from chlorodimethylhydantoin, dichlorodimethylhydantoin, bromodimethylhydantoin, dibromodimethylhydantoin, iododimethylhydantoin, diiododimethylhydantoin, bromochlorodimethylhydantoin, chloroiododimethylhydantoin, and bromoiododimethylhydantoin The coated particle group for producing monohalogenoamine according to <29>, which is a seed or more.

<32>
(D3) Component is from sodium hypochlorite, calcium hypochlorite, magnesium hypochlorite, calcium chloride hypochlorite, magnesium chloride hypochlorite, sodium hypobromite, sodium hypoiodite The coated particle group for producing monohalogenoamine according to <29>, which is one or more selected.

<33>
(D) Component is sodium dichloroisocyanurate, potassium dichloroisocyanurate, trichloroisocyanuric acid, chlorodimethylhydantoin, dichlorodimethylhydantoin, sodium hypochlorite, calcium hypochlorite, magnesium hypochlorite, hypochlorous acid chloride It is a compound selected from calcium acid and magnesium chloride hypochlorite, preferably a compound selected from sodium dichloroisocyanurate, trichloroisocyanuric acid and calcium hypochlorite, more preferably calcium hypochlorite. The coated particle group for producing a monohalogenoamine according to the above <29>.

<34>
The manufacturing method of the covering particle group for monohalogenoamine manufacture which has the following process (1) and (2).
Step (1): (A) Particles of 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 mixed Step of obtaining coated particle group (1) comprising particles of component (A) coated with component (C) Step (2): Coated particle group (1) obtained in step (1) and (B) solid alkali Particles of the component (B) on the component (C) obtained by mixing the particles of the agent (hereinafter referred to as the component (B)) and coating the component (A) of the coated particle group (1) obtained in the step (1) For obtaining a coated particle group (2) comprising particles to which particles adhere

<35>
In step (1), a part or all of component (C) is previously melted and then mixed, preferably, component (C) is melted and then mixed, and the monohalogenoamine production according to <34> above For producing coated particle group for use.

<36>
In 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. More preferably 2 or more, further preferably 2.7 or more, and 6 or less, preferably 5 or less, more preferably 4 or less, and the monohalogeno described in the above <34> or <35> A method for producing a coated particle group for amine production.

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

<38>
In the step (1), when the component (C) is melted and added in advance, the addition rate is 1,000 g / min or less, preferably 600 g / min or less, more preferably 200 g, relative to 100 g of the component (C). / Min or less, more preferably 150 g / min or less, and even more preferably 100 g / min or less, the method for producing a coated particle group for producing monohalogenoamine according to the above <37>.

<39>
In the step (1), mixing is performed using a granulator, and the setting of the fluid number of the granulator defined by the following formula is 50 or less, preferably 40 or less, more preferably 30 or less, and still more preferably 20 The method for producing a coated particle group for producing monohalogenoamine according to any one of the above <34> to <38>, further preferably 10 or less.
Fluid number: Fr = V ² / (R × g)
V: Circumferential 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 vertical or horizontal granulator equipped with main wings and crushing blades, V and R use the values of the main shaft, and in the Nauter mixer in which the stirring unit rotates and revolves, V and R rotate. The value of the stirring shaft will be used. ]

<40>
In 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, according to any one of <34> to <39>. The manufacturing method of the coated particle group for monohalogenoamine manufacture.

<41>
In 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>, wherein the monohalogenoamine is mixed so as to be 1.5 or more, preferably 3 or less, preferably 2.5 or less, more preferably 2 or less. A method for producing a coated particle group for production.

<42>
In the step (2), mixing is performed using a granulator, and the setting of the fluid number of the granulator defined by the above formula is 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>, more preferably 10 or less.

<43>
In step (2), the temperature during mixing is 60 ° C. or higher, preferably 70 ° C. or higher, and 100 ° C. or lower, preferably 90 ° C. or lower, according to any one of <34> to <42>. The manufacturing method of the coated particle group for monohalogenoamine manufacture.

<44>
Furthermore, the manufacturing method of the coated particle group for monohalogenoamine manufacture in any one of said <34>-<43> which has the following process (3).
Step (3): Step of drying the coated particle group (2) obtained in the step (2)

<45>
In step (3), the drying time is 1 hour or longer, preferably 2 hours or longer, more preferably 5 hours or longer, preferably 8 hours or longer, and 24 hours or shorter, preferably 16 hours or shorter, <34 The manufacturing method of the coated particle group for monohalogenoamine manufacture in any one of>-<44>.

<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. The manufacturing method of the coated particle group for monohalogenoamine manufacture in any one of 34>-<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, <34> to <46> The manufacturing method of the coated particle group for monohalogenoamine manufacture in any one of these.

The reagents used in Examples and Comparative Examples are as follows.
(A) Component-Ammonium chloride: Zhuzhou JianhgHai Environment Protection Co. Ltd, average particle size 1mm
(B) Component / calcium hydroxide: manufactured by Iwata Pharmaceutical Co., Ltd., average particle diameter of 20 μm
Component (C): 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, 1,000 according to JISZ8801-1 (established on May 20, 2000, final revised on November 20, 2006). After shaking for 5 minutes using a 400, 1,000, 710, 500, 355, 250, 180, 125, 90, 63, 45 μm sieve, the 50% average diameter is calculated for the sieving mass distribution by the sieving method This was taken as the average particle size. Specifically, 2,000, 1,400, 1,000, 710, 500, 355, 250, 180 of JISZ8801-1 (established on May 20, 2000, final revised on November 20, 2006), Using a sieve of 125, 90, 63, 45 μm, stack in order from a sieve with a small opening on the saucer, add 100 g of the particles from the top of the top 2,000 μm sieve, cover and low tap type sieve Mounted on a shaker (manufactured by HEIKO Mfg. Co., Ltd., tapping 156 times / minute, rolling: 290 times / minute), vibrated for 5 minutes, and then measured the mass of the particles remaining on each sieve and saucer. The mass ratio (%) of the granule above was calculated. The average particle size was determined by accumulating the mass ratios of the particles on the sieve with small openings in order from the saucer, and the total particle size was 50%.

(B) The average particle diameter of a component is the value measured on condition of the following using the laser diffraction / scattering type particle size distribution measuring apparatus (the product made by HORIBA, LA-920).
Solvent: Ethanol Refractive index: 1.2
Circulation speed: 4
Circulation: 3 min

  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 (Fukae Powtech Co., Ltd., volume 2 L), and while stirring under the conditions shown in Table 1, 52.5 g of PEG previously melted at a temperature higher than the melting point was added to 50 g / The mixture was charged at a rate of minutes 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)). Thereafter, 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 having the component (B) attached to the component) was obtained (step (2)). The average particle diameter of the coated particle group (2) was 1,157 μm.

  Moreover, about the covering particle group of Example 1, by observing the surface of (A) component and the surface of covering particle group (2) with an electron microscope (SEM), covering particle group (2) becomes (A) component It was confirmed that the component (B) was adhered to the component (C) coated with a particle structure. 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 the coated particle group (2) was produced under the same conditions as in Example 1, the coated particle group (2) was stored in a desiccator and subjected to a drying treatment at a vacuum degree of 20 kPa abs and a drying temperature of 25 ° C. for 12 hours. The average particle diameter of the coated particle group (2) was 1,160 μm.

Example 3
After the coated particle group (2) was produced under the same conditions as in Example 1, it was sealed 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 the degree of vacuum was 20 kPa abs and dried Drying was performed at a temperature of 25 ° C. for 12 hours. The average particle diameter of the coated particle group (2) was 1,212 μm.

Example 4
A 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 40 ° C. The average particle diameter of the coated particle group (2) was 1,057 μm.

Example 5
After the coated particle group (2) was produced under the same conditions as in Example 1, the coated particle group (2) was stored in an electric dryer (manufactured by ADVANTEC, DRM620TA), and shelf-dried at 50 ° C. for 2 hours in an open state. Processed. The average particle diameter of the coated particle group (2) was 1,175 μm.

Example 6
After the coated particle group (2) was produced under the same conditions as in Example 1, the coated particle group (2) was charged into a fluidized bed (SPIR-A-FLOW manufactured by FREUND), and the flow rate was 50 ° C. and the blowing rate was 3.5 m ^3. / Min for 0.5 hour. The average particle diameter of the coated particle group (2) was 1,166 μm.

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

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

Comparative Example 1
A mixture was obtained by stirring 63.6 g of ammonium chloride and 36.4 g of calcium hydroxide in a beaker using a spatula.

[Evaluation of dissolution time]
In a 1 L beaker, 500 g of ion-exchanged water was added, and the coated particles of the example and the mixture of the comparative example were added 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 confirmed visually 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 suppression of heat generation during component contact]
As component (D), 2.25 g of calcium hypochlorite (Tosoh Co., Ltd. Toyokuron-PTGIII, effective chlorine 70.5%, particle size 2 to 5 mm) and 3.34 g of the mixture of the coated particle group of the example and the comparative example are used. , Put each in a 100 cc polypropylene cup (upper diameter x lower diameter x height: φ60 x φ44 x 74 mm), stir with a glass rod to mix the entire 50 rotation sample per minute, The indicated value of the thermometer one minute after the start of stirring was read with an industrial (ISO) bar-type thermometer), 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 agents]
5 g of each of the coated particle group of the example and the mixture of the comparative example was put into a 200 cc polypropylene cup (upper diameter × lower diameter × height: φ83 × φ58 × 85 mm), smelled by five panelists, and according to the following criteria The intensity of the odor was evaluated by consultation of five panelists. The results are shown in Table 1.
A: Feeling the smell faint B: Feeling the smell a little C: Feeling the smell D: Feeling the smell very strongly, smelling the smell

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

[Monochloramine production evaluation]
It was confirmed that monochloramine was produced by mixing the coated particle group of the example and the mixture of the comparative example with an aqueous sodium hypochlorite solution, respectively.

  In contrast to the examples of the present invention and comparative examples, by combining a solid ammonium salt and a solid alkaline agent into one agent, a monohalogenamine can be easily synthesized in combination with a halogen agent, and the dissolution rate in water is also good. It turns out that it is. Moreover, it turns out that the heat_generation | fever at the time of a solid halogen agent contact is suppressed, and the ammonia smell of the agent is also suppressed.

Claims (7)

  (A) At least a part of particles of a solid ammonium salt (hereinafter referred to as “component (A)”) is coated with (C) a water-soluble binder (hereinafter referred to as “component (C)”). A coated particle group for producing a monohalogenoamine comprising coated particles in which particles of (B) a solid alkaline agent (hereinafter referred to as (B) component) are attached to component (C) coated with.   The coated particle group for producing monohalogenoamine according to claim 1, wherein the mass ratio (A) / (B) of the content of the component (A) and the content of the component (B) is 0.5 or more and 3 or less. .   The coating for monohalogenoamine production according to claim 1 or 2, wherein the mass ratio (A) / (C) of the content of the component (A) and the content of the component (C) is 0.5 or more and 6 or less. Particle group. The manufacturing method of the covering particle group for monohalogenoamine manufacture which has the following process (1) and (2).
Step (1): (A) Particles of 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 mixed Step of obtaining coated particle group (1) comprising particles of component (A) coated with component (C) Step (2): Coated particle group (1) obtained in step (1) and (B) solid alkali Particles of the component (B) on the component (C) obtained by mixing the particles of the agent (hereinafter referred to as the component (B)) and coating the component (A) of the coated particle group (1) obtained in the step (1) For obtaining a coated particle group (2) comprising particles to which particles adhere Furthermore, the manufacturing method of the coated particle group for monohalogenoamine manufacture of Claim 4 which has the following process (3).
Step (3): 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 manufacturing method of the coated particle group for monohalogenoamine manufacture of Claim 4 or 5 mixed with these.   In 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 manufacturing method of the coated particle group for monohalogenoamine manufacture in any one of Claims 4-6 mixed with these.