Powdery pesticidal composition

Abstract

Disclosed is a powdery pesticidal composition which comprises a mixture of a coated pesticide comprising a powdery pesticide coated with a thermosetting resin and having a volume median diameter of 10 to 150 μm and a calcium carbonate micropowder having a bulk density of 0.6 g/ml or less, wherein the weight-based ratio of the coated pesticide to the calcium carbonate micropowder is 100:1 to 100:30. The powdery pesticidal composition has good fluidability.

Claims

1. A powdery pesticidal composition comprising a mixture of a coated pesticide having a volume median diameter of 10 to 150 μm in which a powdery agrichemical is coated with a themosetting resin, and a calcium carbonate micropowder having a bulk density of 0.6 g/ml or less, wherein the weight ratio of the coated pesticide to the calcium carbonate micropowder is in the range of 100:1 to 100:30.

2. The powdery pesticidal composition according to claim 1, wherein the thermosetting resin is a polyurethane resin and/or a polyurea resin.

3. The powdery pesticidal composition according to claim 1 or 2, wherein the bulk density of the calcium carbonate micropowder is in the range of 0.01 to 0.3 g/ml.

4. A method for improving flowability of a powdery coated pesticide which comprises adding a calcium carbonate micropowder having a bulk density of 0.6 g/ml or less to a powdery coated pesticide in which a powdery pesticide is coated with a thermosetting resin, in such an amount that the weight ratio of the powdery coated pesticide and the calcium carbonate micropowder is in the range of 100:1 to 100:30.

Description

EXAMPLES

(1) The present invention will be described in more detail by way of the following Examples which the present invention is not limited to.

Reference Example 1 (Preparation of Coated Pesticide 1)

(2) Preparation of Powdery Pesticide 1:

(3) 70.0 parts by weight of (E)-1-(2-chloro-1,3-thiazol-5-ylmethyl)-3-methyl-2-nitroguanidine (common name: clothianidine) and 30.0 parts by weight of Shokozan Clay S (manufactured by Shokozan Mining Co., Ltd.) were uniformly mixed. The total amount of the mixture was ground with a centrifugation grinding machine to obtain a powdery pesticide having a volume median diameter of 15.0 μm (MASTERSIZER2000 manufactured by MALVERN Instruments Ltd.) and containing (E)-1-(2-chloro-1,3-thiazol-5-ylmethyl)-3-methyl-2-nitroguanidine (hereinafter, referred to as the powdery pesticide 1).

(4) Preparation of Polyol Premix 1

(5) 56.1 parts by weight of SUMIPHEN™ (branched polyether polyol manufactured by Sumika Bayer Urethane Co., Ltd.), 42.3 parts by weight of SUMIPHEN 1600U (linear polyether polyol manufactured by Sumika Bayer Urethane Co., Ltd.) and 1.6 parts by weight of 2,4,6-tris(dimethylaminomethyl)phenol (manufactured by Kayaku Akzo Corporation) were uniformly mixed to obtain a liquid mixture of polyol and a catalyst (hereinafter, referred to as the polyol premix 1). The viscosity of the polyol premix 1 was 364 m.Math.Pa (B-type viscometer, 25° C., 12 rotation, rotor No. 1).

(6) Preparation of Coated Pesticide 1

(7) Into a container of High Speed Mixer apparatus (Model LFS-GS-1J manufactured by Fukae Powtec; an apparatus having agitator blades whose rotation axis is a vertical line passing through the center of the bottom of a round dish-type container part, and chopper blades whose rotation axis is a horizontal line penetrating through the side surface of the round dish-type container part) was loaded 100 parts by weight of the powdery pesticide 1, and the agitator blades (rotation number: 850 rpm) and the chopper blades (rotation number: 3500 rpm) of the apparatus were rotated. Then, the mixing container was warmed, and 1.86 parts by weight of the polyol premix 1 was added thereto while the temperature of the powdery pesticide 1 was kept at 75±5° C. It was observed that the powdery pesticide 1 was wetted with the polyol premix 1. After 3 minutes, 1.14 parts by weight of SUMIDUR 44V10 (polymethylenepolyphenyl polyisocyanate manufactured by Sumika Bayer Urethane Co., Ltd., viscosity 130 m.Math.Pa (25° C.)) was added thereto while the temperature of a product was kept at 75±5° C. From immediately after addition, a phenomenon of viscosity increasing was observed. Thereafter, the viscosity was reduced, and curing of a polyurethane resin was observed (corresponding to 3.0 parts by weight of a polyurethane resin per 100 parts by weight of the powdery pesticide 1). After 5 minutes, the following operation was repeated 19 times while the temperature of a product was kept at 75±5° C.

(8) Addition of 1.86 parts by weight of the polyol premix 1.fwdarw.Wait for 3 minutes.fwdarw.Addition of 1.14 parts by weight of SUMIDUR 44V10.fwdarw.Wait for 5 minutes.

(9) During the above-described operation, the High Speed Mixer apparatus continued stirring and mixing capable of providing a shearing force under the same conditions.

(10) A total of 60 parts by weight of the raw materials of the polyurethane resin were added per 100 parts by weight of the powdery pesticide 1. The mixing container was cooled to obtain the coated pesticide 1 (addition time of raw materials of polyurethane resin: 20 times, addition amount of raw materials of polyurethane resin per one time: 3.0 parts by weight, total addition amount of raw materials of polyurethane resin: 60 parts by weight, volume median diameter: 75 μm, bulk density: 0.41 g/ml).

Reference Example 2 (Preparation of Coated Pesticide 2)

(11) Preparation of Powdery Pesticide 2

(12) 45.5 parts by weight of 5-chloro-N-(1,3-dihydro-1,1,3-trimethyl-4-isobenzofuranyl)-1,3-dimethylpyrazole-4-carboxamide (common name: furametpyr), 9 parts by weight of Tokusil GU-L (hydrous amorphous silicon dioxide manufactured by Tokuyama Corporation) and 45.5 parts by weight of Bentonite Fuji (manufactured by Hojun) were uniformly mixed. The total amount of the mixture was ground with a centrifugation grinding machine to obtain a powdery agrichemical having a volume median diameter of 5.0 μm (MASTERSIZER2000 manufactured by MALVERN Instruments Ltd.) and containing 5-chloro-N-(1,3-dihydro-1,1,3-trimethyl-4-isobenzofuranyl)-1,3-dimethylpyrazole-4-carboxamide (hereinafter, referred to as the powdery pesticide 2).

(13) Preparation of Coated Pesticide 2

(14) Into a container of High Speed Mixer apparatus (Model LFS-GS-1J manufactured by Fukae Powtec; an apparatus having agitator blades whose rotation axis is a vertical line passing through the center of the bottom of a round dish-type container part, and chopper blades whose rotation axis is a horizontal line penetrating through the side surface of the round dish-type container part) was loaded 100 parts by weight of the powdery pesticide 2, and the agitator blades (rotation number: 850 rpm) and the chopper blades (rotation number: 3500 rpm) of the apparatus were rotated. Then, the mixing container was warmed, and 1.86 parts by weight of the polyol premix 1 was added thereto while the temperature of the powdery pesticide 2 was kept at 75±5° C. It was observed that the powdery pesticide 2 was wetted with the polyol premix 1. After 3 minutes, 1.14 parts by weight of SUMIDUR 44V10 (polymethylenepolyphenyl polyisocyanate manufactured by Sumika Bayer Urethane Co., Ltd., viscosity 130 m.Math.Pa (25° C.)) was added thereto while the temperature of a product was kept at 75±5° C. From immediately after addition, a phenomenon of viscosity increasing was observed. Thereafter, the viscosity was reduced, and curing of a polyurethane resin was observed (corresponding to 3.0 parts by weight of a polyurethane resin per 100 parts by weight of the powdery pesticide). After 5 minutes, the following operation was repeated 6 times while the temperature of a product was kept at 75±5° C.

(15) Addition of 1.86 parts by weight of the polyol premix 1.fwdarw.Wait for 3 minutes.fwdarw.Addition of 1.14 parts by weight of SUMIDUR 44V10.fwdarw.Wait for 5 minutes.

(16) During the above-described operation, the High Speed Mixer apparatus continued stirring and mixing capable of providing a shearing force under the same conditions.

(17) A total of 21 parts by weight of the raw materials of the polyurethane resin were added per 100 parts by weight of the powdery pesticide 2. The mixing container was cooled to obtain the coated pesticide 2 (addition time of raw materials of polyurethane resin: 7 times, addition amount of raw materials of polyurethane resin per one time: 3.0 parts by weight, total addition amount of raw materials of polyurethane resin: 21 parts by weight, volume median diameter: 40 μm, bulk density: 0.37 g/ml).

Reference Example 3 (Preparation of Coated Pesticide 3)

(18) Preparation of Powdery Pesticide 3

(19) 65 parts by weight of (E)-N-(6-chloro-3-pyridylmethyl)-N-ethyl-N′-methyl-2-nitrovinylidenediamine (common name: nitenpyram) and 35 parts by weight of Shokozan Clay S (kaolin clay: manufactured by Shokozan Mining Co., Ltd.) were uniformly mixed. The total amount was ground with a centrifugation grinding machine to obtain a powdery agrichemical having a volume median diameter of 16.0 μm (MASTERSIZER2000 manufactured by MALEVRN Instruments Ltd.) and containing (E)-N-(6-chloro-3-pyridylmethyl)-N-ethyl-N′-methyl-2-nitrovinylidenediamine (hereinafter, referred to as the powdery pesticide 3).

(20) Preparation of Coated Pesticide 3

(21) Into a container of High Speed Mixer apparatus (Model LFS-GS-1J manufactured by Fukae Powtec; an apparatus having agitator blades whose rotation axis is a vertical line passing through the center of the bottom of a round dish-type container part, and chopper blades whose rotation axis is a horizontal line penetrating through the side surface of the round dish-type container part) was loaded 100 parts by weight of the powdery pesticide 3, and the agitator blades (rotation number: 1800 rpm) and the chopper blades (rotation number: 2000 rpm) of the apparatus were rotated. Then, the mixing container was warmed, and 1.55 parts by weight of the polyol premix 1 was added thereto while the temperature of the powdery pesticide 3 was kept at 75±5° C. It was observed that the powdery pesticide 3 was wetted with the polyol premix 1. After 3 minutes, 0.95 parts by weight of SUMIDUR 44V10 (polymethylenepolyphenyl polyisocyanate manufactured by Sumika Bayer Urethane Co., Ltd., viscosity 130 m.Math.Pa (25° C.)) was added thereto while the temperature of a product was kept at 75±5° C. From immediately after addition, a phenomenon of viscosity increasing was observed. Thereafter, the viscosity was reduced, and curing of a polyurethane resin was observed (corresponding to 2.5 parts by weight of a polyurethane resin per 100 parts by weight of the powdery pesticide). After 5 minutes, the following operation was repeated 19 times while the temperature of a product was kept at 75±5° C.

(22) Addition of 1.55 parts by weight of the polyol premix 1.fwdarw.Wait for 3 minutes.fwdarw.Addition of 0.95 parts by weight of SUMIDUR 44V10.fwdarw.Wait for 5 minutes.

(23) During the above-described operation, the High Speed Mixer apparatus continued stirring and mixing capable of providing a shearing force under the same conditions.

(24) A total of 50 parts by weight of the raw materials of the polyurethane resin were added per 100 parts by weight of the powdery pesticide 3. The mixing container was cooled to obtain the coated pesticide 3 (addition time of raw materials of polyurethane resin: 20 times, addition amount of raw materials of polyurethane resin per one time: 2.5 parts by weight, total addition amount of raw materials of polyurethane resin: 50 parts by weight, volume median diameter: 53 μm).

Preparation Examples 1 to 12 and Comparative Examples 1 to 6 (Preparation of Powdery Composition)

(25) The coated pesticide 1 prepared in Reference Example 1 and a micropowder described in the following Table 1 were charged into a container of High Speed Mixer apparatus (Model LFS-GS-1J manufactured by Fukae Powtec) at the weight ratio described in Table 1. The materials were stirred and mixed by rotating agitator blades (rotation number: 850 rpm) and chopper blades (rotation number: 3500 rpm) of the apparatus for 5 minutes to prepare a powdery composition.

(26) TABLE-US-00001 TABLE 1 Coated Apparent pesticide specific 1:micropowder Micropowder gravity (g/ml) (weight ratio) Production Calcium carbonate (*1) 0.25 100:4 Example 1 Production Calcium carbonate (*1) 0.25 100:7 Example 2 Production Calcium carbonate (*1) 0.25  100:10 Example 3 Production Calcium carbonate (*2) 0.24 100:4 Example 4 Production Calcium carbonate (*2) 0.24 100:7 Example 5 Production Calcium carbonate (*2) 0.24  100:10 Example 6 Production Calcium carbonate (*3) 0.38 100:4 Example 7 Production Calcium carbonate (*3) 0.38 100:7 Example 8 Production Calcium carbonate (*3) 0.38  100:10 Example 9 Production Calcium carbonate (*4) 0.53 100:4 Example 10 Production Calcium carbonate (*4) 0.53 100:7 Example 11 Production Calcium carbonate (*4) 0.53  100:10 Example 12 Comparative Pyrophyllite (*5) 0.65 100:4 Example 1 Comparative Pyrophyllite (*5) 0.65 100:7 Example 2 Comparative Pyrophyllite (*5) 0.65  100:10 Example 3 Comparative Calcium carbonate (*6) 0.91 100:4 Example 4 Comparative Calcium carbonate (*6) 0.91 100:7 Example 5 Comparative Calcium carbonate (*6) 0.91  100:10 Example 6 (*1): Light calcium carbonate (manufactured by Maruo Calcium Co., Ltd.) (*2): Heavy calcium carbonate NS#2300 (manufactured by Nitto Funka Kogyo K.K.) (*3): Heavy calcium carbonate NS#400 (manufactured by Nitto Funka Kogyo K.K.) (*4): Heavy calcium carbonate SS#80 (manufactured by Nitto Funka Kogyo K.K.) (*5): Shokozan Clay S (hydrous aluminum silicate; manufactured by Shokozan Mining Co., Ltd.) (*6): Heavy calcium carbonate NN#200 (manufactured by Nitto Funka Kogyo K.K.)

(27) Then, flowability of the above-prepared pesticidal compositions was assessed by the following test method. Each test result is described in Table 2.

(28) Here, the test was performed using a powder tester Model PT-D (manufactured by Hosokawa Micron Group).

Test Example 1 (Spatula Angle)

(29) A vat was placed on a ramp for measuring a spatula angle, and a sample was added thereto until the spatula was hidden. The ramp was calmly lowered, and a tilt angle of a side surface of the sample accumulated on the spatula was measured (tilt angle 1). Then, an attached bell was used to make an impact on the spatula, and a tilt angle of a side surface of the sample accumulated on the spatula was measured (tilt angle 2). An average of the tilt angle 1 and the tilt angle 2 was adopted as a spatula angle.

(30) TABLE-US-00002 TABLE 2 Tilt angle 1 Tilt angle 2 Average (degree) (degree) (degree) Only coated 90 90 90 pesticide 1 Production 80 65 73 Example 1 Production 64 46 55 Example 2 Production 60 50 55 Example 3 Production 70 50 60 Example 4 Production 59 47 53 Example 5 Production 50 42 46 Example 6 Production 70 56 63 Example 7 Production 64 50 57 Example 8 Production 55 44 50 Example 9 Production 76 60 68 Example 10 Production 72 54 63 Example 11 Production 62 49 56 Example 12 Comparative 90 82 86 Example 1 Comparative 90 82 86 Example 2 Comparative 90 62 76 Example 3 Comparative 90 76 83 Example 4 Comparative 90 80 85 Example 5 Comparative 90 64 77 Example 6

INDUSTRIAL APPLICABILITY

(31) The powdery pesticidal composition of the present invention has good flowability as a powder, and is useful as a composition containing a coated pesticide in which a powdery pesticide is coated with a thermosetting resin.