A soluble granule containing dinotefuran and preparation method thereof

Abstract

The present invention relates to a soluble granule containing dinotefuran and a preparation method thereof, and belongs to the technical field of pesticides. A soluble granule containing dinotefuran, wherein the soluble granule contains the following components in percentage by mass: 5% to 60% dinotefuran; 1% to 5% wetting agent; 2% to 10% binder; and 25% to 92% carrier. Compared with the traditional basket extrusion granulation, the preparation method of the present invention is easier to produce particles for the above formula, and has the beneficial effect of using a limited space to instantly heat up and soften the material, screw extrusion, and cooling into dense particles, which reduces hygroscopicity, regular particles, simple process, low energy consumption, safety and environmental protection.

Description

Technical Field

[0001] The invention relates to a soluble granule containing dinotefuran and a preparation method thereof, belonging to the technical field of pesticides. Background Art

[0002] Dinotefuran, chemically known as 1-methyl-2-nitro-3-(tetrahydro-3-furanmethyl)guanidine, is a third-generation nicotinoid insecticide developed by Mitsui Chemicals, Japan. Its main mechanism of action is to interfere with the neurotransmission system of insects. By binding to acetylcholine receptors, it disrupts nerve signal transmission, causing insects to become abnormally excited, convulse, and even paralyzed and die. In the preparation of soluble granules, the industry generally uses soluble salts such as sodium acetate, urea phosphate, and sodium chloride as fillers to obtain good granulation and dissolution effects. However, these soluble salts usually have strong hygroscopicity, especially in the extrusion granulation process. Due to the increase in temperature, their hygroscopicity is further enhanced, which brings challenges to the traditional extrusion granulation process. Specifically, it manifests itself in serious bonding and clogging problems, which affect the smooth progress of the granulation process. To overcome this problem, some manufacturers choose to abandon the use of sodium acetate, which has strong hygroscopicity, as a filler and instead use organic salt fillers with lower hygroscopicity, such as sodium benzoate and sodium citrate. Other manufacturers choose to granulate in a closed environment where humidity and temperature can be precisely controlled. Although this method can use traditional fillers such as sodium acetate and sodium chloride, it requires huge equipment investment and high energy consumption. Summary of the invention

[0003] The purpose of the present invention is to address the defects of the prior art and to provide a soluble granule containing dinotefuran and a preparation method thereof. The material is softened by instantaneous heating in a limited space, and a screw is extruded and cooled into dense particles, thereby reducing hygroscopicity and making the particles regular. At the same time, due to the simplicity of the equipment, the production cost is reduced.

[0004] The present invention solves the technical problem through the following technical scheme: firstly, a soluble granule containing dinotefuran is provided, wherein the soluble granule contains the following components in percentage by mass: 5% to 60% of dinotefuran; 1% to 5% of a wetting agent; 2% to 10% of a binder; and 25% to 92% of a carrier.

[0005] The wetting agent in the above components is a sulfonate anion with good dissolution rate and hot melt softening ability, and the sulfonate is selected from at least one of linear sodium dodecylbenzene sulfonate (LAS), branched sodium dodecylbenzene sulfonate (BAS), C1416 α-olefin sulfonate (C1416AOS), secondary alkyl sodium sulfonate (SAS) and sodium hexadecyl diphenyl ether disulfonate (8390), and triethylenetetramine type sulfonate.

[0006] Furthermore, the wetting agent is triethylenetetramine sulfonate, with a content of 2% to 3%.

[0007] The binder is at least one of sucrose, glucose, sorbitol, mannitol, lactose, xylitol and maltitol.

[0008] Furthermore, the binder is at least one of sucrose, mannitol, lactose and maltitol.

[0009] Furthermore, the binder is one of mannitol and lactose, with a content of 4% to 8%. The granulation is particularly excellent in the dissolution, clarity and granulation process.

[0010] The carrier is at least one of sodium chloride, sodium acetate and urea phosphate.

[0011] Furthermore, the carrier is sodium acetate.

[0012] The invention provides a method for preparing soluble granules containing dinotefuran with low energy consumption and simple process to meet the requirements of customers and solve the difficulties of traditional granulation process, as well as the high energy consumption of traditional granulation process. The process is relatively complicated and needs to be mixed, crushed, kneaded with water, extruded granulated, dried, granulated and screened. The method comprises the following steps: evenly mixing 5% to 60% of dinotefuran, 1% to 5% of a wetting agent, 2% to 10% of a binder and 25% to 92% of a carrier, and then mechanically crushing the mixture, adding the mixture into a fully automatic hot melt granulator (with a cooling system) for granulation, and then hot melting and screw extrusion granulation are carried out inside the equipment, and the finished particles are cut and cooled.

[0013] Granulation principle: crush the material, mix it evenly, add it to the equipment, heat it and soften it, extrude it through the screw, cut it into particles by the cutter at the extruder, and cool it down with cold air at the outlet before entering the large package. The particle size can be controlled by the screen and the cutter movement frequency.

[0014] Granulation process of dinotefuran soluble granules: 1. Mix all materials according to the formula and crush them mechanically to control the particles below 65 microns. 2. Set the heating temperature at 65℃~120℃, preferably 85℃~95℃; select the sieve with an aperture of 1.2mm, adjust the screw operation frequency to 35HZ, the discharge cooling air temperature is less than 10℃, the wind speed is 10m / s, and the cutter movement frequency is 1s / time, which is adjusted according to the size of the particles. 3. When the heating chamber is stable at more than 65℃, add the crushed mixed powder, and the mixed powder enters the heating chamber through the screw movement. The heated material is soft and sticky, and then squeezed out of the sieve by screw extrusion. It is cooled by the wind passing through the outlet and hardens instantly. It is cut by the movement of the cutter to become the desired particle size.

[0015] Compared with traditional basket extrusion granulation, the preparation method of the present invention is easier to produce particles for the above formula. Its beneficial effects are that the material is softened by instantaneous heating in a limited space, and the screw is extruded and cooled into dense particles, which reduces hygroscopicity, regular particles, simple process, low energy consumption, safety and environmental protection. DETAILED DESCRIPTION

[0016] The following examples are in terms of mass percentage: Dinotefuran soluble granules, dinotefuran: 5%~60%; wetting agent: 1%~5%; binder: 2%~10%; carrier: 25%~92%.

[0017] The wetting agents are linear sodium dodecylbenzene sulfonate (LAS), branched sodium dodecylbenzene sulfonate (BAS), C1416 alpha-olefin sulfonate (C1416AOS), secondary sodium alkyl sulfonate (SAS) and sodium hexadecyl diphenyl ether disulfonate (8390), triethylenetetramine type sulfonate.

[0018] The binders are sucrose, glucose, sorbitol, mannitol, lactose, xylitol and maltitol.

[0019] The carriers are sodium chloride, sodium acetate and urea phosphate.

[0020] Granulation process of dimethoate soluble granules: 1. Mix all materials according to the formula and crush them mechanically to control the particles below 65 microns. 2. Set the heating temperature at 65°C to 120°C, preferably 85°C to 95°C; select a 1.2 mm aperture for the screen, adjust the screw operating frequency to 35HZ, the discharging cooling air temperature is less than 10°C, the wind speed is 10m / s, and the cutter movement frequency is 1s / time, which is adjusted according to the size of the particles. 3. When the heating bin is stably greater than 65°C, add the crushed mixed powder, which enters the heating bin through the movement of the screw. The heated material is a soft and sticky material, which is then extruded from the screen by screw extrusion. It is cooled by the wind passing through the outlet and instantly hardened. It is cut by the movement of the cutter to become the desired particle size. The following embodiments are granulated according to the above method and will not be repeated. Embodiment 1

[0021] 15% dinotefuran soluble granules: dinotefuran 15%, linear sodium dodecylbenzene sulfonate 4%, xylitol 10%, urea phosphate 71%; 15% dinotefuran soluble granules are obtained through mixing, crushing, hot-melt granulation and cooling. Embodiment 2

[0022] 20% dinotefuran soluble granules: dinotefuran 20%, triethylenetetramine sulfonate 3%, mannitol 8%, sodium acetate 69%; 20% dinotefuran soluble granules are obtained by mixing, crushing, hot-melt granulation and cooling. Embodiment 3

[0023] 30% dinotefuran soluble granules: 30% dinotefuran, 3% sodium cetyl diphenyl ether disulfonate, 8% maltitol, 59% sodium acetate; 30% dinotefuran soluble granules are obtained by mixing, crushing, hot-melt granulation and cooling. Embodiment 4

[0024] 40% dinotefuran soluble granules: dinotefuran 40%, triethylenetetramine sulfonate 3%, lactose 8%, sodium chloride 49%; 40% dinotefuran soluble granules are obtained through mixing, crushing, hot-melt granulation and cooling.

[0025] The samples of the prepared dinotefuran soluble granules in Examples 1 to 4 above were taken for efficacy testing.

[0026] The control agents were commercially available 40% dinotefuran soluble granules A and B.

[0027] The efficacy test (cockroach cylinder) is shown in Table 1: Table 1

[0028] The above tests show that the dinotefuran soluble granules prepared by the above formula and process are comparable to market samples in terms of efficacy, and the preparation method is simpler, with obvious cost reduction and efficiency improvement.

[0029] In addition to the above implementations, the present invention may also have other implementations. Any technical solution formed by equivalent replacement or equivalent transformation falls within the protection scope required by the present invention.

Claims

1. A soluble granule containing dinotefuran, characterized in that: The soluble granules contain the following components in percentage by mass: 5% to 60% of dinotefuran; 1% to 5% of a wetting agent; 2% to 10% of a binder; and 25% to 92% of a carrier.

2. The soluble granules containing dinotefuran according to claim 1, characterized in that: The wetting agent is a sulfonate anion, and the sulfonate is selected from at least one of linear sodium dodecylbenzene sulfonate (LAS), branched sodium dodecylbenzene sulfonate (BAS), C1416 α-olefin sulfonate (C1416AOS), secondary alkyl sodium sulfonate (SAS), sodium hexadecyl diphenyl ether disulfonate (8390), and triethylenetetramine type sulfonate.

3. The soluble granules containing dinotefuran according to claim 2, characterized in that: The wetting agent is triethylenetetramine sulfonate, with a content of 2% to 3%.

4. The soluble granules containing dinotefuran according to claim 1, characterized in that: The binder is at least one of sucrose, glucose, sorbitol, mannitol, lactose, xylitol and maltitol.

5. The soluble granules containing dinotefuran according to claim 4, characterized in that: The binder is at least one of sucrose, mannitol, lactose and maltitol.

6. The soluble granules containing dinotefuran according to claim 5, characterized in that: The binder is one of mannitol and lactose, with a content of 4% to 8%.

7. The soluble granules containing dinotefuran according to claim 1, characterized in that: The carrier is at least one of sodium chloride, sodium acetate and urea phosphate.

8. The soluble granules containing dinotefuran according to claim 7, characterized in that: The carrier is sodium acetate.

9. A method for preparing a soluble granule containing dinotefuran, characterized in that: After 5% to 60% of dinotefuran, 1% to 5% of wetting agent, 2% to 10% of binder and 25% to 92% of carrier are uniformly mixed, the mixture is heated and softened in a hot melt chamber, extruded into granules and cooled to obtain the finished product.

10. The method for preparing the soluble granules containing dinotefuran according to claim 9, characterized in that: After mixing all the components evenly, they are mechanically crushed and the particles are controlled below 65 microns; the heating temperature is 65℃~120℃; the screen has an aperture of 1.2 mm, the screw operating frequency is 35HZ, the discharge cooling air temperature is less than 10℃, the wind speed is 10m / s, and the cutter movement frequency is 1s / time; when the heating chamber is stably greater than 65℃, the crushed mixed powder is added, and the mixed powder enters the heating chamber through the movement of the screw. The heated material becomes soft and sticky, and is then extruded from the screen by screw extrusion, and then cooled by the outlet wind, instantly hardened, and cut by the movement of the cutter to obtain particles of the target size.

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