JP2003146804A - Granular wettable powder for disinfecting seed with high-concentration dilution - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a granular wettable powder for disinfecting seeds with high-concentration dilution comprising an agrochemically active ingredient without causing precipitates or having good redispersibility of the precipitates even if the precipitates are formed when the high-concentration diluted liquid is prepared. SOLUTION: This wettable powder for disinfecting the seeds with the high- concentration dilution comprises the agrochemically active ingredient, a nonionic surfactant and/or an anionic surfactant, bentonite having >=10 ml/2 g swelling power and a glassy powder composed of fragments of an irregular shape obtained by pulverizing a natural glassy foam.

Description

Detailed Description of the Invention

[0001]

TECHNICAL FIELD The present invention relates to a granular wettable powder for disinfecting highly concentrated diluted seeds, which has good disintegrating property and redispersibility.

[0002]

2. Description of the Related Art Conventionally, since wettable powders are fine powdery preparations, there have been problems such as scattering of fine powders during production and preparation of drug solutions, and complexity of drug measurement. Therefore, in order to solve these problems, attempts have been made to granulate and granulate wettable powders. Examples include: [Patent Document 1] JP-A-8-143403 DISCLOSURE OF THE INVENTION Problems to be Solved by the Invention The average particle size of the irregularly shaped particles obtained by crushing the agricultural chemical active ingredient and natural glassy foam has an average particle size of 5 to 10.
Granular agrochemical wettable powder containing 0 μm vitreous powder, JP-A-9-301801, pesticide active ingredient, average particle size of irregularly shaped particles obtained by crushing natural vitreous foam. 5 μm to 10
Agrochemical granular wettable powder containing 0 μm vitreous powder, lauryl sulfate, anionic surfactant other than lauryl sulfate, binder, and solid carrier, JP-A-2000-204001, bentonite, natural vitreous foam The average particle size of the irregularly-shaped fine particles obtained by crushing
A granular pesticide wettable powder containing 0 μm vitreous powder.

On the other hand, in order to disinfect a large amount of seeds with a chemical,
The seed disinfectant is diluted with, for example, 3 to 20 times by weight of water to form a diluting solution (hereinafter, referred to as "high-concentration diluting liquid"), and a high-concentration diluting liquid in an amount corresponding to 3% of dry seed weight is prepared. A method of spraying seeds using a spray device for seed disinfection has become widespread.

However, when a conventional granular pesticide wettable powder is diluted with water to prepare a high-concentration diluting solution and seed disinfection work is performed with a seed disinfecting spraying device, the flow of the chemical liquid in the chemical liquid tank or spraying device is reduced. A large amount of sediment forms hard caking in the channel, blocking the channel and making it difficult to clean the lower part of the chemical liquid tank and the channel at the end of the work.

[0005]

As described above, the existing granular pesticide wettable powder is not always satisfactory in terms of redispersibility of the precipitate formed when it is used as a high-concentration diluted solution. Therefore, development of a granular pesticide wettable powder capable of preparing a high-concentration diluted solution without such a defect is desired.

Accordingly, an object of the present invention is to provide a granular wettable powder for disinfecting highly concentrated diluted seeds, which does not cause precipitation when a highly concentrated diluent is prepared, or has good redispersibility of the precipitate even when it occurs. To provide.

[0007]

[Means for Solving the Problems] The inventors of the present invention have conducted extensive studies to solve these problems. As a result, pesticide active ingredients, nonionic surfactants and / or anionic surfactants, bentonite with a swelling power of 10 ml / 2 g or more, irregular shapes obtained by crushing natural glassy foams Granular pesticide wettable powder containing vitreous powder consisting of fine particles, the redispersibility at the time of preparing a high-concentration diluted solution is better than the conventional granular pesticide wettable powder, solving the above-mentioned problems. The present invention has been completed by finding out that

In the present invention, it is important to pulverize the natural glassy foam body into irregularly shaped pieces, and the average particle size of such pieces is 5 to 100 μm.
m, but preferably 5 μm to 80 μm
m, more preferably, by pulverizing into fine particles having an average particle size of 10 to 30 μm, individual particles become irregularly shaped fine particles and keep the density of particles at the time of granulation low, A pesticide formulation having good disintegration and dispersibility can be obtained.

On the other hand, when a granular wettable powder is prepared in an attempt to prepare a high-concentration diluting solution using an unground product of natural glassy foam, and when this is diluted with water, particles of the wettable powder are formed on the water surface. It floats, does not disperse well in water, and has poor suspension.

Therefore, in the present invention, the natural glassy foam is crushed to obtain an average particle size of 5 to 100 μm.
It is important that the powder has a particle size of m, preferably 5 μm to 80 μm, more preferably 10 μm to 30 μm.

Conventionally, when bentonite is used,
The particles of the granular wettable powder had a drawback that the particles became hard and the disintegration property was extremely poor. However, by using a glassy powder having an average particle diameter of 5 to 100 μm obtained by crushing a natural glassy foam together with bentonite,
It is possible to obtain an agrochemical formulation having improved disintegration property and good redispersibility of the precipitate generated over time. in this case,
In particular, it has been found that when bentonite having a swelling power of 10 ml / 2 g or more is used, the redispersibility of the high-concentration diluted solution is significantly improved.

In the conventional wettable powder for pesticides, a large amount of sediment causes hard caking when diluted to a high concentration. However, when bentonite having a swelling power of 10 ml / 2 g or more is used as in the present invention, this swelling is caused. Hard caking does not occur due to the force, and it becomes a soft agglomerate sediment, which is easily redispersed by weak stirring. And the swelling power is 10 ml / 2
With bentonite having a swelling power of g or less and having a low swelling power, when a high-concentration diluted solution is prepared, the resulting precipitate is hard and the redispersibility is insufficient. When bentonite having a swelling power of 40 ml / 2 g or more is used, the thickening power of bentonite exerts a large effect this time, resulting in poor disintegration. Therefore, the swelling power is 10
It is desirable to use ~ 40 ml / 2g bentonite.

[0013]

BEST MODE FOR CARRYING OUT THE INVENTION Next, a method for carrying out the granular wettable powder for disinfecting highly diluted seeds of the present invention will be specifically described.

The pesticidal active ingredient used in the granular wettable powder for disinfecting highly concentrated diluted seeds of the present invention is a pesticide used for controlling seed diseases such as rice bark seedling disease and rice sesame leaf blight, and pest control by seed disinfection. It may be any active ingredient. Moreover, you may use together 1 type, or 2 or more types of these agricultural chemical active ingredients.

Examples of such pesticidal active ingredients include the following, but the pesticidal active ingredients applicable in the present invention are not limited to these examples.

Sterilizing active ingredient benomyl for seed disinfection, thiabendazole, thiophanate methyl,
Thiuram, prochloraz, trifumizole, ipconazole, basic copper chloride, cupric hydroxide, etc.

Insecticidal active ingredient for seed disinfection Fenitrothion etc.

The amount of these agrochemical active ingredients added to the preparation is not particularly limited, but generally 0.1 to 90% by weight, preferably 1 to 80% by weight of the total preparation.
Is.

The names of these pesticidal active ingredients are the common names described in "Agricultural Chemical Handbook 1998 Edition" (published by the Japan Plant Protection Association, December 15, 1998).

As the bentonite used in the present invention, sodium bentonite whose main component is montmorillonite (main component is sodium montmorillonite), calcium bentonite (main component is calcium montmorillonite), and purified bentonite (high-purity sodium) Montmorillonite), and its swelling power is 10 ml / 2 g or more. This is because when bentonite having a swelling power of 10 ml / 2 g or less is used, redispersibility after diluting the granular wettable powder with water is poor. Further, a granular wettable powder using bentonite having a swelling power of 40 ml / 2 g or more has poor disintegration property in water. Therefore, it is desirable to use bentonite having a swelling power of 10 to 40 ml / 2 g in the present invention.

In the present invention, as long as bentonite having such requirements is used, there is no problem even if one kind or two or more kinds are used in combination, and the amount added to the preparation is 1 to 30% by weight. The range is good.

The powder obtained by crushing the natural glassy foam of the present invention is derived from natural glassy materials such as obsidian, pearlite and shale, and shirasu, but those derived from pearlite and shirasu are more preferable. desirable. Further, the powder obtained by crushing these glassy foams is a sintered perlite and shirasu balloon or a commercially available product obtained by heating and foaming a natural glassy substance by an ordinary method, and an average particle diameter by an ordinary pulverizer. It is crushed to 5 to 100 μm. When the particle size of the powder obtained by crushing the glassy foam exceeds 100 μm, the hardness of the particles after granulation becomes weak,
There are problems such as easy pulverization, disintegration in water, and poor dispersibility. Further, when the average particle diameter is less than 5 μm, it is also related to the granulation means, but generally the hardness of the particles after granulation becomes strong and the disintegration property in water becomes poor. Therefore, the average particle size should be 5 μm or more and 100 μm or less, preferably 5 to 80 μm, and more preferably 10 to 30 μm.

The powder obtained by crushing such a natural glassy foam does not pose any problem even if one kind or a combination of two or more kinds is used, and 2% by weight or more, preferably 20 to 20% by weight in the preparation.
It is preferable to add 70% by weight.

As the nonionic surfactant used in the present invention, polyoxyethylene alkyl ether, polyoxyethylene alkylaryl ether, polyoxyethylene styryl phenyl ether, polyoxyethylene alkyl ester, polyoxyethylene sorbitan alkylate. , Polyoxyethylene phenyl ether polymer, polyoxyethylene alkylene aryl phenyl ether, polyoxyethylene alkylene glycol, polyoxyethylene / polyoxypropylene block polymer, fluorine-based surfactant (perfluoroalkylcarboxylic acid, etc.), silicone-based surfactant Agents (polyoxyalkylene dimethyl polysiloxane copolymer, etc.), acetylene glycol-based surfactants (2, 4, 7, 9,-
Tetramethyl-decyne-4,7-diol, etc.), but are not limited to these examples.

There is no problem even if one or more such nonionic surfactants are used in combination, and the HLB of such nonionic surfactants is preferably 10 to 16,
It is more preferably 12 to 15. The amount of addition is preferably 0.1 to 20% by weight in the preparation.

As the anionic surfactant used in the present invention, lignin sulfonate, alkylaryl sulfonate, dialkyl sulfosuccinate, polyoxyethylene alkyl aryl ether sulfate, alkyl naphthalene sulfonate, alkyl naphthalene. Formalin condensate of sulfonic acid, polyoxyethylene styryl phenyl ether sulfate, alkylbenzene sulfonate, alkyl sulfate, and the like are included, but not limited to these examples.

There is no problem even if one or more such anionic surfactants are used in combination, and the addition amount is preferably 0.1 to 30% by weight in the preparation from the viewpoint of effect and economy. It is preferably 0.3 to 20% by weight in the preparation.

In the present invention, there is no problem even if these nonionic surfactants and anionic surfactants are used in combination.

Further, in the present invention, if necessary, generally used binders, antiseptic / antifungal agents, stabilizers for agrochemical active ingredients, and extenders such as inorganic carriers and organic carriers can be used.

In the present invention, a binder is used when the hardness of the granular wettable powder is desired. The binder may be any conventionally used one, for example, natural products derived from cellulose, methyl cellulose, ethyl cellulose, carboxymethyl cellulose, hydroxymethyl cellulose, hydroxyethyl cellulose, hydroxypropyl cellulose, starch, carboxymethyl starch, pullulan, alginic acid. Sugar-based substances such as sodium, ammonium alginate, dextran, mannan, pectin, tragacanth gum, mannitol, sorbitol, propylene glycol alginate guar gum, locust bean gum, gum arabic or xanthan gum, and protein-based substances such as gelatin and casein. Synthetic substances include polyvinyl alcohol, polyethylene oxide, polyethylene glycol. Le, ethylene-propylene block polymer, sodium polyacrylate, polyvinyl pyrrolidone, and the like.

The kind of the binder and the amount thereof to be used should be determined in consideration of the desired disintegrating property of the granular wettable powder of the present invention. 0.1 to 40% by weight is desirable.

Examples of the antiseptic / antifungal agents that can be used include sorbic acid, potassium sorbate, parachloro-metaxylenol, butyl paraoxybenzoate, and the like. As stabilizers for pesticide active ingredients, antioxidants and ultraviolet ray inhibitors are used. If desired, a crystal precipitation preventing agent may be added.

Examples of the inorganic carrier used in the present invention include clay, talc, calcium carbonate, sodium carbonate, sikhlite, sericite, acid clay, silica stone, diatomaceous earth, pumice stone, zeolite, vermiculite and white carbon. And examples of organic carriers include saw iron, straw,
There are monosaccharides such as pulp, chaff, glucose, fructose, sucrose, maltose, lactose, starch and dextrin, disaccharides and polysaccharides.

[0034]

EXAMPLES The granular wettable powder for disinfecting highly concentrated diluted seeds of the present invention can be easily prepared by the method described below.

That is, the pesticide active ingredient, the nonionic surfactant and / or the anionic surfactant, and the swelling power is 10
ml / 2g or more of bentonite, powder mixture composed of glassy powder consisting of irregularly shaped fine particles obtained by crushing natural glassy foam, if necessary, a binder, inorganic Alternatively, it is mixed with an organic carrier, an antiseptic / antifungal agent, a stabilizer of an agrochemical active ingredient, etc., and is kneaded with water and granulated using an extrusion granulator, followed by drying and sizing.

In consideration of handling convenience and disintegration property of the preparation, it is generally preferable to appropriately adjust the particle size in the range of 0.1 to 10 mm. Further, while adding water to the powder mixture, it may be granulated by a tumbling granulator, dried and sized. Further, the powder mixture may be dispersed in water and produced by a spray-drying granulator. Alternatively, the powder mixture may be fluidized and sprayed with an aqueous binder solution or the like to produce a fluidized bed granulator. No problem at all.

Next, the present invention will be described in more detail with reference to examples, but the present invention is not limited thereto. All "parts" below refer to parts by weight.

Example 1 20 parts of benomyl, 5 parts of polyoxyethylene styryl phenyl ether (HLB = 10.0), 4 parts of sodium dodecylbenzene sulfonate, 4 parts of sodium salt of β-naphthalene sulfonic acid formalin condensate, swelling power 28 ml /
10.0 parts of 2 g of sodium bentonite (trade name "Kunigel VA" manufactured by Kunimine Industries Co., Ltd.), powder obtained by crushing natural glassy foam derived from pearlite (a product manufactured by Mitsui Mining & Smelting Co., Ltd. Name "Roca help B409", average particle size 13 μm) 47.0 parts and sucrose 10 parts were mixed with a hammer mill (manufactured by Fuji Paudal Co., Ltd.), and then 25 parts of water was added to 100 parts of this mixture, and double arms Knead and mix with a kneader (manufactured by Fuji Paudal Co., Ltd.). Then 0.6
Granulation is carried out by an extrusion granulator (manufactured by Nippon Pharmaceutical Co., Ltd.) equipped with a screen having a diameter of mm, further dried by a fluidized bed dryer (manufactured by Fuji Paudal Co., Ltd.) and sieved to give a particle size of 0.25 to 0.25 0.
71 mm of granular wettable powder for disinfecting highly concentrated seeds was obtained.

Example 2 Example 1 was carried out by substituting the polyoxyethylene styryl phenyl ether of Example 1 (HLB = 10.0) with the polyoxyethylene styryl phenyl ether of HLB = 14.0.
Was prepared according to.

Example 3 20 parts benomyl, 20 parts thiuram, 4 parts sodium dodecylbenzenesulfonate, 4 parts sodium salt of β-naphthalenesulfonic acid formalin condensate, swelling power 28 ml /
10.0 parts of 2 g of sodium bentonite (trade name "Kunigel VA" manufactured by Kunimine Industries Co., Ltd.), powder obtained by crushing natural glassy foam derived from pearlite (a product manufactured by Mitsui Mining & Smelting Co., Ltd. After mixing 32.0 parts of "Roca help B409", an average particle diameter of 13 μm) and 10 parts of sucrose with a hammer mill, 20 parts of water is added to 100 parts of this mixture and kneaded and mixed with a double-arm kneader. Next, 0.6m
Granulated by an extrusion granulator equipped with a m-diameter screen, further dried by a fluidized bed dryer and sieved to give a particle size of 0.25 to 0.
71 mm of granular wettable powder for disinfecting highly concentrated seeds was obtained.

Example 4 Basic copper chloride 8 parts, sodium dodecylbenzene sulfonate 4 parts, sodium salt of β-naphthalene sulfonic acid formalin condensate 4 parts, swelling power 28 ml / 2 g of sodium bentonite (Kunimine Industries Co., Ltd.) Trade name "Kunigel VA") 10.0 parts, powder obtained by crushing natural glassy foam derived from pearlite (trade name "Rocahelp B409" manufactured by Mitsui Mining & Smelting Co., Ltd., average particle diameter 13 μm) 5
After mixing 9.0 parts and 15 parts of sucrose with a hammer mill,
To 100 parts of this mixture, 25 parts of water is added, and the mixture is kneaded and mixed with a twin-arm kneader. Next, it is granulated by an extrusion granulator equipped with a screen of 0.6 mm diameter, further dried by a fluidized bed dryer and then sieved to disinfect highly concentrated diluted seeds having a particle diameter of 0.25 to 0.71 mm. A granular wettable powder was obtained.

Example 5 20 parts of benomyl, 4 parts of sodium dodecylbenzene sulfonate, 4 parts of sodium salt of β-naphthalene sulfonic acid formalin condensate, swelling power of 28 ml / 2 g of sodium bentonite (trade name of Kunimine Industries Co., Ltd.) "Kunigel V
A ”) 20.0 parts, powder obtained by crushing natural glassy foam derived from pearlite (trade name“ Rocahelp B409 ”manufactured by Mitsui Mining & Smelting Co., Ltd., average particle diameter 13 μm) 4
After mixing 2.0 parts and 10 parts of sucrose with a hammer mill,
20 parts of water is added to 100 parts of this mixture, and the mixture is kneaded and mixed with a double-arm kneader. Next, it is granulated by an extrusion granulator equipped with a screen of 0.6 mm diameter, further dried by a fluidized bed dryer and then sieved to disinfect highly concentrated diluted seeds having a particle diameter of 0.25 to 0.71 mm. A granular wettable powder was obtained.

Example 6 20 parts of benomyl, 4 parts of sodium dodecylbenzene sulfonate, 4 parts of a sodium salt of a β-naphthalene sulfonic acid formalin condensate, and a high-purity sodium montmorillonite having a swelling power of 65 ml / 2 g (Kunimine Industries Co., Ltd.) Product name "Kunipia G") 10.0 parts, powder obtained by crushing natural glassy foam derived from pearlite (product name "Rocahelp B409" manufactured by Mitsui Mining & Smelting Co., Ltd., average particle size 13)
(5 μm) and 10 parts of sucrose are mixed with a hammer mill, 25 parts of water is added to 100 parts of this mixture, and the mixture is kneaded and mixed with a double-arm kneader. Next, granulation is carried out by an extrusion granulator equipped with a screen having a diameter of 0.6 mm, further dried by a fluidized bed dryer and sieved to obtain a particle size of 0.25 to 0.71.
A granular wettable powder for disinfecting highly concentrated diluted seeds of mm was obtained.

Example 7 The high-purity sodium montmorillonite of Example 6 was swelled at 6
It was prepared according to Example 6 by substituting 0 ml / 2 g of high-purity sodium montmorillonite (trade name “Kunipia F” manufactured by Kunimine Industries Co., Ltd.).

Comparative Example 1 The high-purity sodium montmorillonite of Example 6 was swelled at 7
Example 6 substituting 2 ml of calcium bentonite (trade name "Kunibond" manufactured by Kunimine Industries Co., Ltd.)
Was prepared according to.

Comparative Example 2 The sodium bentonite of Example 5 was swelled at 7 ml / 2 g.
It was prepared according to Example 5 by substituting the calcium bentonite (trade name: “Kunibond” manufactured by Kunimine Industries Co., Ltd.).

Next, with respect to the granular wettable powder for disinfecting highly-concentrated diluted seeds of the present invention, a test example for evaluating the disintegration property when poured into water and the redispersibility of the precipitate generated upon dilution with water will be shown. .

Test Example 1 Disintegration test 90 ml of 3 degree hard water at 20 ° C. was placed in a cylinder with a capacity of 100 ml, and 13.33 g of a granular wettable powder for disinfecting highly concentrated diluted seeds was added to the bottom of the cylinder. The cylinder was inverted 1 minute after reaching, and the number of inversions until all the particles collapsed was counted. The results are shown in Table 1.

Test Example 2 Redispersibility test 13.33 g of a granular wettable powder for disinfecting highly concentrated diluted seeds was placed in a 100 ml capacity cylinder with a stopper, and tap water was added to add 1
Make up the volume to 00 ml. The cylinder was inverted 40 times and inverted to prepare a high concentration diluted solution. This is left to stand in a constant temperature water bath at 10 ° C. for 48 hours. Then, the cylinder is repeatedly inverted and the number of inversions required for the precipitate to be completely redispersed in water is determined. The results are shown in Table 1.

Test Example 3 Flow Path Closure Test 100 with a chemical solution outlet drawn by a magnet pump in the center of the bottom and a circulating chemical solution inlet at the top
10 kg of a granular wettable powder for disinfecting high-concentration seeds is placed in a liter-capacity poly tank (first tank), and tap water is added to prepare a high-concentration diluent of 75 liters. Another 7-liter capacity poly tank (second tank) is connected by using a magnet pump connected to the chemical solution outlet by a pipe, and is installed so as to circulate the chemical solution in the two poly tanks. This chemical solution is circulated at a rate of 2 liters / minute. During the circulation of the chemical liquid, the chemical liquid in the first tank is stirred using a stirrer.

After being circulated for 6 hours in this way, a glass rod having a diameter of 5 mm, a length of 25 cm and a weight of 10 g was dropped perpendicularly to the sediment from 10 cm above the sediment formed in the second tank. Then, the hardness of the sediment was evaluated in two stages, in which the glass rod pierces the sediment and is soft when the glass rod reaches the bottom of the tank and is hard when the glass rod does not reach the bottom of the tank. In this case, if the generated sediment is hard, there is a high possibility that the flow path of the pipe will be blocked when the seed disinfecting chemical is sprayed on the seed. After that, a chemical solution is poured onto the sediment in the second tank at a flow rate of 2 liters / minute, and the sediment is redispersed in a good cleaning property, and if it is not redispersed, the cleaning property is inferior. did. The results are shown in Table 1.

The swelling power of bentonite in the present invention is determined by the following method (a method based on the bentonite swelling power test method of the 13th Revised Japanese Pharmacopoeia).

A 2.0 g sample was taken and added to a 100 ml capacity graduated cylinder with a ground-in stopper in 100 ml of purified water in 10 batches. However, after most of the previously added sample is deposited, the next sample is added. When the addition of the sample is completed, the sample is capped and allowed to stand at room temperature for 24 hours, and the apparent volume (ml) of the sample accumulated in the container is read.

[0054]

INDUSTRIAL APPLICABILITY The granular wettable powder for disinfecting highly concentrated diluted seeds of the present invention has good disintegration property even when a highly concentrated diluted liquid is prepared, and the precipitate formed is soft and easy to clean. Good redispersibility.

[0055]

[Table 1]

   ─────────────────────────────────────────────────── ─── Continued front page    F-term (reference) 4H011 AA01 BA01 BA05 BA06 BB13                       BB14 BB18 BC07 BC18 BC19                       BC20 DA02 DA15 DC05 DC06                       DC08 DD03 DG16 DH03

Claims (4)

[Claims] 1. A pesticide active ingredient, a nonionic surfactant and / or an anionic surfactant, having a swelling power of 10 ml / 2.
Granular wettable powder for disinfecting highly-concentrated diluted seeds, characterized in that it contains bentonite in an amount of g or more and vitreous powder consisting of irregularly-shaped fine particles obtained by crushing natural vitreous foam. . 2. The granular wettable powder for disinfecting highly concentrated diluted seeds according to claim 1, wherein bentonite having a swelling power of 10 to 40 ml / 2 g is used. 3. The granular wettable powder for disinfecting highly concentrated diluted seeds according to claim 1, wherein the vitreous powder has an average particle size of 5 to 100 μm. 4. The nonionic surfactant has an HLB of 10 to 1.
6. The granular wettable powder for disinfecting highly concentrated diluted seeds according to claim 1, wherein the granular wettable powder of claim 6 is used.