Fluazinam and ethyl acetate suspension agent, and preparation method and application thereof

Abstract

The present application relates to the technical field of pesticide composition, especially to the field of IPC A01N 43, more particularly to a flonicamid and ethyl acetate suspension agent, and a preparation method and application thereof. The components include: ethyl acetate 5-20%, flonicamid 20-40%, dispersant 4-15%, auxiliary agent 1-12%, and deionized water to make up the balance. The weight ratio of ethyl acetate and flonicamid is 1:(1-5), which can improve the efficacy of the suspension agent, so that it can be applied to the control of mites in cotton, flowers, vegetables, fruit trees; the dispersant includes carboxylate dispersant and comb polymer, and the weight ratio of the carboxylate dispersant and the comb polymer is 1:(0.2-2), which can avoid the creaming of the prepared suspension agent particles, the particle size analysis of the particles, and the skinning phenomenon; the carboxylate dispersant is selected from Agrilan 788, and the comb polymer is selected from Agrilan 755, which can improve the stability of the particle size of the suspension agent particles after heat storage, and avoid the increase of the particle size after heat storage.

Description

Technical Field

[0001] This invention relates to the field of pesticide composition technology, particularly to the field of IPCA01N43, and more specifically, to a suspension concentrate of fluazinam and etoxazole, its preparation method and application. Background Technology

[0002] Throughout the history of pesticide development, the mixed use of pesticides has always been an integral part of pesticide evolution. Typically, a highly effective commercial pesticide is accompanied by numerous related mixtures, and the market value created by mixtures often exceeds that of single-agent pesticides. Continuous use of insecticides containing a single active ingredient can easily lead to pesticide resistance in pests. By mixing insecticides with two active ingredients in a specific ratio to create a mixture, efficacy can often be improved, the amount of active ingredient required can be reduced, costs can be saved, and the development of pesticide resistance in pests can be delayed.

[0003] Chinese invention patent CN108013044A discloses a pesticide composition containing fluazinam and etoxazole. The active ingredients are fluazinam and etoxazole. The dispersant used in the suspension formulation includes one or more of the following: polycarboxylate, formaldehyde condensate of sodium methylnaphthalene sulfonate, sodium lignosulfonate, calcium lignosulfonate, p-methoxy fatty amide benzenesulfonic acid, desaccharified and fractionated sodium lignosulfonate, sodium salt of naphthalene sulfonic acid condensate, sodium salt of alkylnaphthalene sulfonic acid condensate, and formaldehyde condensate of alkylphenol polyoxyethylene ether, etc. This patent does not investigate the stability of the suspension formulation, and the poor stability of the suspension itself is a problem that urgently needs to be solved. Summary of the Invention

[0004] The first aspect of the present invention provides a suspension of fluazinam and etoxazole, comprising, by weight percentage: 5-20% etoxazole, 20-40% fluazinam, 4-15% dispersant, 1-12% adjuvant, and deionized water to make up the balance.

[0005] The additives include at least one of antifreeze, thickener, defoamer and preservative.

[0006] Preferably, the additives include antifreeze, thickener, defoamer, and preservative.

[0007] The antifreeze agent includes at least one of ethylene glycol, propylene glycol, glycerol, and urea.

[0008] The thickener includes at least one of magnesium aluminum silicate, sodium benzoate, xanthan gum, polyvinyl alcohol, and sodium alginate.

[0009] Preferably, the thickener comprises magnesium aluminum silicate and xanthan gum, wherein the weight ratio of magnesium aluminum silicate to xanthan gum is (3-8):1.

[0010] More preferably, the weight ratio of magnesium aluminum silicate to xanthan gum is (3-5):1.

[0011] Preferably, the thickener further includes propylene glycol alginate, and the amount of propylene glycol alginate added to the suspending agent is 0.1-0.5%.

[0012] The defoamer includes at least one of silicone defoamers and polyether defoamers.

[0013] Preferably, the defoamer includes an organosilicone defoamer.

[0014] More preferably, the defoamer includes at least one of defoamer DF-830, defoamer 1572, and defoamer DF-1108.

[0015] The preservative includes at least one of parabens, 1,2-benzisothiazolin-3-one, isothiazolinone, and sodium benzoate.

[0016] Preferably, the components, by weight percentage, include: 5-20% etoxazole, 20-40% fluazinam, 4-15% dispersant, 1-8% antifreeze, 0.1%-2% thickener, 0.01-0.5% defoamer, 0.01-0.5% preservative, and deionized water to make up the balance.

[0017] More preferably, the components, by weight percentage, include: 8-20% etoxazole, 20-40% fluazinam, 4-12% dispersant, 3-8% antifreeze, 0.5%-2% thickener, 0.01-0.1% defoamer, 0.01-0.1% preservative, and deionized water to make up the balance.

[0018] The weight ratio of etoxazole and fluazinam is 1:(1-5).

[0019] Preferably, the weight ratio of etoxazole to fluazinam is 1:(2-4).

[0020] The dispersant includes at least one of carboxylate dispersants, sulfonate dispersants, and comb polymers.

[0021] The dispersant comprises a carboxylate dispersant and a comb-like polymer, wherein the weight ratio of the carboxylate dispersant to the comb-like polymer is 1:(0.2-2).

[0022] Preferably, the weight ratio of the carboxylate dispersant to the comb-like polymer is 1:(1-2).

[0023] More preferably, the weight ratio of the carboxylate dispersant to the comb-like polymer is 1:(1.2-2).

[0024] The carboxylate dispersants include polyacid salt dispersants.

[0025] Preferably, the polyacid salt dispersant includes at least one of the following models from J&R Technology: Agrilan 700, Agrilan 789, Agrilan 785, and Agrilan 788.

[0026] The comb-like polymer includes anionic comb-like polymers.

[0027] Preferably, the side chain repeating units of the anionic comb polymer include at least one of ethylene glycol, propylene glycol, and butanediol.

[0028] More preferably, the side chain repeating unit of the anionic comb polymer includes propylene glycol, preferably Agrilan 755 from Jerun Technology.

[0029] A second aspect of this invention provides a method for preparing a suspension of fluazinam and etoxazole, comprising the following steps:

[0030] Step 1: Mix deionized water, comb-like polymer, and additives evenly to obtain a mixture;

[0031] Step 2: Add etoxazole and fluazinam to the mixture, mix well, then add a carboxylate dispersant, mix well, and the product is obtained.

[0032] A weight ratio of tebufenozide to fluazinam of 1:(1-5) can improve the efficacy of the suspension, making it applicable to the control of mites on cotton, flowers, vegetables, and fruit trees. However, at this weight ratio, the dispersibility of tebufenozide and fluazinam is poor. This application's research found that the dispersant comprises a carboxylate dispersant and a comb-like polymer, with a weight ratio of 1:(0.2-2). This avoids the formation of paste-like particles, particle separation during sieving, and crusting in the prepared suspension particles. This may be a combination of two dispersants in a specific ratio, which can increase the thickness of the electric double layer on the particle surface and the steric hindrance of the macromolecular chains, thereby solving the problem of flocculation between suspension particles and making the formulation more stable.

[0033] Further research in this application revealed that selecting Agrilan 788 as a carboxylate dispersant and Agrilan 755 as a comb polymer can improve the stability of the suspension particle size after heat storage and avoid particle size growth after heat storage. This may be due to the interaction between the hydrophilic and hydrophobic functional groups of Agrilan 788 and the polypropylene glycol side chains of Agrilan 755. At the same time, the weak anionic groups on the molecular chain of Agrilan 755 provide additional electrostatic repulsion, which improves the wettability of the suspension particles and ensures the dispersibility of the active ingredient.

[0034] However, the carboxylate dispersant Agrilan 788 can cause the drug solution to turn red during use, thus affecting the apparent properties of the suspension. This application has found by chance that adding the carboxylate dispersant Agrilan 788 to the system after adding etoxazole and fluazinam can solve the problem of the drug solution turning red. This may be because there is an interaction or chemical reaction between Agrilan 788 and fluazinam, and the specific order of addition reduces the specific surface area of ​​contact between Agrilan 788 and fluazinam.

[0035] Based on the system of this invention, magnesium aluminum silicate and xanthan gum in a mass ratio of (3-8):1 are used as thickeners, which solves the problem of particle precipitation after thermal storage and further improves the stability of thermal storage. The applicant believes that the reason may be that under the specific composition and compounding ratio of thickener, the viscosity of the suspension system is adjusted, the precipitation rate of etoxazole and fluazinam suspension particles in the system is reduced, the precipitation stratification phenomenon is reduced, the thixotropic fluidity of the suspension is improved, and the interaction between the two components in a specific ratio makes the suspension more stable.

[0036] The third aspect of this invention provides an application of fluazinam and etoxazole suspension for the control of mites in cotton, flowers, vegetables, and fruit trees.

[0037] The mites include at least one of the following: spider mite, early spider mite, and carmine spider mite.

[0038] Beneficial effects

[0039] 1. The weight ratio of etoxazole and fluazinam is 1:(1-5), which can improve the efficacy of the suspension and make it applicable to the control of mites in cotton, flowers, vegetables and fruit trees.

[0040] 2. The dispersant includes a carboxylate dispersant and a comb-like polymer, wherein the weight ratio of the carboxylate dispersant to the comb-like polymer is 1:(0.2-2), which can avoid the formation of paste, particle separation, and skin formation in the prepared suspension particles.

[0041] 3. Selecting Agrilan 788 as a carboxylate dispersant and Agrilan 755 as a comb polymer can improve the stability of the suspension particle size after heat storage and avoid particle size growth after heat storage.

[0042] 4. Using magnesium aluminum silicate and xanthan gum in a mass ratio of (3-8):1, along with propylene glycol alginate as a thickener, solves the problem of particle precipitation after heat storage, further improving heat storage stability. At the same time, the addition of propylene glycol alginate can also play a physical sealing role against red spider mites, reducing the development of resistance and improving efficacy.

[0043] 5. The carboxylate dispersant Agrilan 788 is added to the system after etoxazole and fluazinam are added to the mixture. It can inhibit the oxidation of fluazinam and solve the problem of reddening of the drug solution. Attached Figure Description

[0044] Figure 1 The results are from the particle size test before thermal storage in Example 1.

[0045] Figure 2 The results are from the particle size test after thermal storage in Example 1.

[0046] Figure 3 This is a visual representation of the product after thermal storage in Example 1.

[0047] Figure 4 The above is the apparent graph of Comparative Example 1 at room temperature.

[0048] Figure 5 The above is the apparent graph at room temperature for Comparative Example 2.

[0049] Figure 6 The images show the appearance of Example 1 and Comparative Example 4 at room temperature, with the left image corresponding to Comparative Example 4 and the right image corresponding to Example 1. Detailed Implementation

[0050] Example 1

[0051] A suspension concentrate containing fluazinam and etoxazole, comprising, by weight percentage: etoxazole 10.6%, fluazinam 32.1%, dispersant 8%, adjuvant 4.82%, and deionized water to make up the balance.

[0052] The dispersants include Agrilan 755 and Agrilan 788.

[0053] A method for preparing a suspension of fluazinam and etoxazole comprises the following steps:

[0054] Step 1: Add 89.18g of deionized water, 10g of Agrilan 755 (comb polymer, Jierun Technology), and 9.66g of additives to a shearing kettle and shear until homogeneous to obtain a mixture.

[0055] Step 2: Add 21.23g of etoxazole (Kechuang, technical grade, 98.9wt%) and 64.26g of fluazinam (Youjia, technical grade, 98wt%) to a shearing vessel and shear for 20 minutes. Then add 6g of Agrilan 788 (carboxylate dispersant, Jierun Technology) and shear for 10 minutes. Finally, grind the uniform shearing liquid in a sand mill. After passing the wet sieve test, the product is obtained.

[0056] The additives include: 8g propylene glycol (antifreeze), 1.5g thickener, 0.3g 1,2-benzisothiazolin-3-one (preservative, Shangwei Chemical, active ingredient 20wt%) and 0.06g defoamer 1572 (defoamer).

[0057] The thickener is a compound of magnesium aluminum silicate, xanthan gum and propylene glycol alginate, wherein the weight ratio of magnesium aluminum silicate to xanthan gum is 10:3:2.

[0058] Comparative Example 1

[0059] A suspension concentrate containing fluazinam and etoxazole, comprising, by weight percentage: etoxazole 10.6%, fluazinam 32.1%, dispersant 8%, adjuvant 4.82%, and deionized water to make up the balance.

[0060] The dispersants include Agrilan 755 and Morwet D-500.

[0061] A method for preparing a suspension of fluazinam and etoxazole comprises the following steps:

[0062] Step 1: Add 89.18g of deionized water, 10g of Agrilan 755 (comb polymer, Jierun Technology), 6g of MORWETD-500 (alkyl naphthalene sulfonate sodium, Jierun Technology), and 9.66g of additives to a shearing kettle and shear them until they are mixed evenly to obtain a mixture.

[0063] Step 2: Add 21.23g of etoxazole (Kechuang, technical grade, 98.9wt%) and 64.26g of fluazinam (Youjia, technical grade, 98wt%) to the shearing vessel, shear for 30 minutes, then grind the uniform shearing liquid with a sand mill, and after passing the wet sieve test, the product is obtained.

[0064] The additives include: 8g propylene glycol (antifreeze), 1.5g thickener, 0.3g 1,2-benzisothiazolin-3-one (preservative, Shangwei Chemical, active ingredient 20wt%) and 0.06g defoamer 1572 (defoamer).

[0065] The thickener is a compound of magnesium aluminum silicate, xanthan gum and propylene glycol alginate, wherein the weight ratio of magnesium aluminum silicate to xanthan gum is 10:3:2.

[0066] Comparative Example 2

[0067] A suspension concentrate containing fluazinam and etoxazole, comprising, by weight percentage: etoxazole 10.6%, fluazinam 32.1%, dispersant 8%, adjuvant 4.82%, and deionized water to make up the balance.

[0068] The dispersants include Agrilan 755 and Morwet D-425.

[0069] A method for preparing a suspension of fluazinam and etoxazole comprises the following steps:

[0070] Step 1: Add 89.18g of deionized water, 10g of Agrilan 755 (comb polymer, Jierun Technology), 6g of MORWETD-425 (alkyl naphthalene sulfonate formaldehyde condensate, Jierun Technology), and 9.66g of additives to a shearing kettle and shear them until they are mixed evenly to obtain a mixture.

[0071] Step 2: Add 21.23g of etoxazole (Kechuang, technical grade, 98.9wt%) and 64.26g of fluazinam (Youjia, technical grade, 98wt%) to the shearing vessel, shear for 30 minutes, then grind the uniform shearing liquid with a sand mill, and after passing the wet sieve test, the product is obtained.

[0072] The additives include: 8g propylene glycol (antifreeze), 1.5g thickener, 0.3g 1,2-benzisothiazolin-3-one (preservative, Shangwei Chemical, active ingredient 20wt%) and 0.06g defoamer 1572 (defoamer).

[0073] The thickener is a compound of magnesium aluminum silicate, xanthan gum and propylene glycol alginate, wherein the weight ratio of magnesium aluminum silicate to xanthan gum is 10:3:2.

[0074] Comparative Example 3

[0075] A suspension concentrate containing fluazinam and etoxazole, comprising, by weight percentage: etoxazole 10.6%, fluazinam 32.1%, dispersant 8%, adjuvant 4.82%, and deionized water to make up the balance.

[0076] The dispersants include Agrilan 755 and Agrilan 788.

[0077] A method for preparing a suspension of fluazinam and etoxazole comprises the following steps:

[0078] Step 1: Add 89.18g of deionized water, 10g of Agrilan 755 (comb polymer, Jierun Technology), 6g of Agrilan 788 (carboxylate dispersant, Jierun Technology), and 9.66g of additives to a shearing kettle and shear until homogeneous to obtain a mixture.

[0079] Step 2: Add 21.23g of etoxazole (Kechuang, technical grade, 98.9wt%) and 64.26g of fluazinam (Youjia, technical grade, 98wt%) to the shearing vessel, shear for 30 minutes, then grind the uniform shearing liquid with a sand mill, and after passing the wet sieve test, the product is obtained.

[0080] The additives include: 8g propylene glycol (antifreeze), 1.5g thickener, 0.3g 1,2-benzisothiazolin-3-one (preservative, Shangwei Chemical, active ingredient 20wt%) and 0.06g defoamer 1572 (defoamer).

[0081] The thickener is a compound of magnesium aluminum silicate, xanthan gum and propylene glycol alginate, wherein the weight ratio of magnesium aluminum silicate to xanthan gum is 10:3:2.

[0082] Performance testing methods

[0083] The suspensions prepared in the examples and comparative examples were subjected to the following tests, and the test data are listed in Table 1, where "-" indicates no experiment was conducted.

[0084] 1. Appearance properties of suspension: At room temperature, observe with the naked eye whether there are phenomena such as sanding into paste, sieving out particles or crystals, forming a skin, or the liquid turning red. If none of the above phenomena are present, it is qualified; otherwise, it is unqualified.

[0085] 2. D90 particle size test: room temperature test.

[0086] 3. Thermal storage performance test: thermal storage at 54℃ for 2 weeks, followed by testing of apparent performance and D90 particle size.

[0087] Performance test data

[0088] Table 1

[0089]

[0090] like Figure 1 and Figure 2 As shown, in Example 1, the particle size hardly increased after 2 weeks of heat storage, as... Figure 3 As shown, in Example 1, after two weeks of heat storage, sieve analysis revealed no particles or crystals, and no residue adhering to the wall. Figure 4-5 As shown, using a dispersant other than the preferred one will result in paste formation, particle separation on sieves, and skin formation, etc. Figure 6 As shown, if an alternative preparation method is used, the liquid will turn red.

Claims

1. A suspension concentrate containing fluazinam and etoxazole, characterized in that, The components, by weight percentage, include: 5-20% etoxazole, 20-40% fluazinam, 4-15% dispersant, 1-12% adjuvants, and deionized water to make up the balance; the weight ratio of etoxazole to fluazinam is 1:(1-5). The dispersant includes carboxylate dispersants and comb-like polymers; The weight ratio of the carboxylate dispersant to the comb-like polymer is 1:(0.2-2); the carboxylate dispersant is Agrilan 788; the comb-like polymer is Agrilan 755; The additives include at least one of antifreeze, thickener, defoamer and preservative; the thickener includes propylene glycol alginate, magnesium aluminum silicate and xanthan gum; the magnesium aluminum silicate and xanthan gum are compounded in a weight ratio of (3-8):1; The method for preparing the fluazinam and etoxazole suspension is characterized by comprising the following steps: Step 1: Mix deionized water, comb-like polymer, and additives evenly to obtain a mixture; Step 2: Add etoxazole and fluazinam to the mixture, mix well, then add a carboxylate dispersant, mix well, and the product is obtained.

2. An application of the fluazinam and etoxazole suspension according to claim 1, characterized in that, It is used for mite control in cotton, flowers, vegetables, and fruit trees.

Images