Fluazinam and SYP-9625 suspending agent as well as preparation method and application thereof

Abstract

The invention relates to the technical field of pesticide compositions, in particular to the field of IPC A01N 43, and more particularly relates to a fluazinam and SYP-9625 suspending agent as well as a preparation method and application thereof. The composition comprises the following components: 5-20% of SYP-9625, 20-40% of fluazinam, 4-15% of a dispersant, 1-12% of an auxiliary agent and the balance of deionized water. The weight ratio of the SYP-9625 to the fluazinam is 1: (1-5), so that the pesticide effect of the suspending agent can be improved, and the suspending agent can be applied to mite prevention and control of cotton, flowers, vegetables and fruit trees; the dispersing agent comprises a carboxylate dispersing agent and a comb-shaped polymer, the weight ratio of the carboxylate dispersing agent to the comb-shaped polymer is 1: (0.2-2), and the phenomena that particles of the prepared suspending agent are pasty, particles exist after screening out and crusting occurs can be avoided; the carboxylate dispersing agent selects Arilan 788, and the comb-shaped polymer selects Arilan 755, so that the stability of the particle size of the suspending agent particles after heat storage can be improved, and the increase of the particle size after heat storage is avoided.

Description

Technical Field

[0001] The present invention relates to the technical field of pesticide compositions, in particular to the field of IPCA01N43, and more specifically to a fluazinam and ethidium sulfaquinoxaline suspension concentrate and a preparation method and application thereof. Background Art

[0002] In the history of the development of pesticides, the mixed use of pesticides has always been developed along with the development of pesticides. Usually, a commercial variety with excellent effects will be accompanied by many related mixed varieties, and the market value created by the mixed varieties is often greater than that of single-dose varieties. Pesticides containing a single active ingredient are easily used in pest control to cause pests to develop resistance. By mixing two active ingredient pesticides into mixed components in a certain proportion, it is often possible to improve the prevention effect, reduce the amount of active ingredients, save costs, and delay the development of pest resistance.

[0003] Chinese invention patent CN108013044A discloses a pesticide composition containing fluazinam and ethidium pyrifos, wherein the active ingredients are fluazinam and ethidium pyrifos, and the dispersant used in the suspension formulation includes one or more of polycarboxylates, formaldehyde condensate of sodium methyl naphthalene sulfonate, sodium lignin sulfonate, calcium lignin sulfonate, p-methoxy fatty amide benzene sulfonic acid, desugared and graded sodium lignin sulfonate, sodium salt of naphthalene sulfonic acid condensate, sodium salt of alkyl naphthalene sulfonic acid polycondensate, sulfuric acid of formaldehyde condensate of alkylphenol polyoxyethylene ether, etc. The patent does not explore the stability of the suspension formulation, and the poor stability of the suspension agent of the composition itself is a problem that needs to be solved urgently. Summary of the invention

[0004] The first aspect of the present invention provides a fluazinam and ethiophanate suspension, which comprises, by weight percentage, 5-20% ethiophanate, 20-40% fluazinam, 4-15% dispersant, 1-12% auxiliary agent, and the balance is made up of deionized water.

[0005] The auxiliary agent includes at least one of an antifreeze agent, a thickener, a defoaming agent and a preservative.

[0006] Preferably, the auxiliary agents include antifreeze agents, thickeners, defoaming agents and preservatives.

[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, and the weight ratio of magnesium aluminum silicate to xanthan gum is (3-8):1.

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

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

[0012] The defoaming agent includes at least one of an organosilicon defoaming agent and a polyether defoaming agent.

[0013] Preferably, the defoaming agent comprises a silicone defoaming agent.

[0014] Further preferably, the defoaming agent includes at least one of defoaming agent DF-830, defoaming agent 1572, and defoaming agent DF-1108.

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

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

[0017] Further preferably, the components include, by weight percentage: 8-20% of ethidium bromide, 20-40% of fluazinam, 4-12% of dispersant, 3-8% of antifreeze agent, 0.5%-2% of thickener, 0.01-0.1% of defoamer, 0.01-0.1% of preservative, and the balance is made up of deionized water.

[0018] The weight ratio of ethidium bromide to fluazinam is 1:(1-5).

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

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

[0021] The dispersant comprises a carboxylate dispersant and a comb-like polymer, and 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 polymer is 1:(1-2).

[0023] More preferably, the weight ratio of the carboxylate dispersant to the comb 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 of Jierun Technology: Agrilan 700, Agrilan 789, Agrilan 785, and Agrilan 788.

[0026] The comb polymer includes anionic comb polymer.

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

[0028] Further preferably, the side chain repeating units of the anionic comb polymer include propylene glycol, preferably Agrilan 755 from Jerun Technology.

[0029] The second aspect of the present invention provides a method for preparing a suspension concentrate of fluazinam and ethidium bromide, comprising the following steps:

[0030] Step 1, mixing deionized water, a comb polymer and an additive to obtain a mixture;

[0031] Step 2, adding ethazofenil and fluazinam to the mixture, mixing evenly, and then adding a carboxylate dispersant, mixing evenly to obtain the product.

[0032] The weight ratio of ethidium bromide and fluazinam is 1:(1-5), which can improve the efficacy of the suspension, so that it can be used for the control of mites in cotton, flowers, vegetables, and fruit trees, but the dispersibility of ethidium bromide and fluazinam is poor at this weight ratio. The present application found that the dispersant includes a carboxylate dispersant and a comb-like polymer, and the weight ratio of the carboxylate dispersant and the comb-like polymer is 1:(0.2-2), which can avoid the paste, granules on screening, and crusting of the prepared suspension particles. It may be a combination of two dispersants in a specific ratio, which can increase the double layer thickness on the particle surface and the steric hindrance of the macromolecular chain, thereby solving the problem of flocculation between the suspensions and making the preparation more stable.

[0033] Further research in this application found that the selection of Agrilan 788 as a carboxylate dispersant and Agrilan 755 as a comb polymer can improve the stability of the particle size of the suspension after thermal storage and avoid the growth of the particle size after thermal 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 original drug.

[0034] However, during the use of the carboxylate dispersant Agrilan 788, the drug solution may turn red, which in turn affects the apparent performance of the suspension concentrate. The present applicant accidentally discovered that the carboxylate dispersant Agrilan 788 can solve the problem of the drug solution turning red by adding it to the system after ethidium bromide and fluazinam are added to the mixture. This may be due to the 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 the present invention, magnesium aluminum silicate and xanthan gum with a mass ratio of (3-8): 1 are used as thickeners to solve the problem of particle precipitation after hot storage and further improve the hot storage stability. The applicant analyzed that the reason may be: under a specific thickener composition and compounding ratio, the viscosity of the suspension system is adjusted, the precipitation rate of the ethoxyfenocic acid and fluazinam suspension particles in the system is reduced, the precipitation stratification phenomenon is reduced, the thixotropic fluidity of the suspension is improved, and under the interaction between the two components in a specific ratio, the suspension becomes more stable.

[0036] The third aspect of the present invention provides an application of a fluazinam and ethazifop suspension, which is applied to the control of mites in cotton, flowers, vegetables and fruit trees.

[0037] The mites include at least one of spider mites, early spider mites, and cinnabarinus spider mites.

[0038] Beneficial Effects

[0039] 1. The weight ratio of ethidium bromide and fluazinam is 1:(1-5), which can improve the efficacy of the suspension concentrate 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 prevent the prepared suspension particles from becoming creamy, having particles on screening, and forming a skin.

[0041] 3. Select Agrilan 788 as carboxylate dispersant and Agrilan 755 as comb polymer to improve the stability of the particle size of the suspension after hot storage and avoid the increase of particle size after hot storage.

[0042] 4. The use of aluminum magnesium silicate and xanthan gum in a mass ratio of (3-8):1 and the addition of propylene glycol alginate as thickeners solves the problem of particle precipitation after hot storage and further improves the hot storage stability. At the same time, the addition of propylene glycol alginate can also play a physical sealing role on red spider mites, reduce the development of resistance, and improve the efficacy.

[0043] 5. The carboxylate dispersant Agrilan 788 is added to the system after ethidium bromide and fluazinam are added to the mixture. It can inhibit the oxidation of fluazinam and solve the problem of redness of the drug solution. BRIEF DESCRIPTION OF THE DRAWINGS

[0044] Figure 1 This is the particle size test result before thermal storage in Example 1.

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

[0046] Figure 3 This is the appearance diagram after heat storage of Example 1.

[0047] Figure 4 This is the appearance diagram of Comparative Example 1 at room temperature.

[0048] Figure 5 This is the appearance diagram of Comparative Example 2 at room temperature.

[0049] Figure 6 These are the appearance diagrams of Example 1 and Comparative Example 4 at room temperature, wherein the left diagram corresponds to Comparative Example 4, and the right diagram corresponds to Example 1. DETAILED DESCRIPTION

[0050] Example 1

[0051] A fluazinam and ethiophanate suspension comprises the following components by weight: 10.6% of ethiophanate, 32.1% of fluazinam, 8% of a dispersant, 4.82% of an auxiliary agent, and the balance is made up of deionized water.

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

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

[0054] Step 1, 89.18 g of deionized water, 10 g of Agrilan 755 (comb polymer, Jierun Technology), and 9.66 g of additives were added into a shearing kettle and sheared and mixed uniformly to obtain a mixture;

[0055] Step 2, add 21.23g of ethazolin (Ke Chuang, technical content 98.9wt%) and 64.26g of fluazinam (Youjia, technical content 98wt%) into the shearing kettle, shear for 20min, then add 6g of Agrilan 788 (carboxylate dispersant, Jierun Technology), shear for 10min, and then grind the uniform shear liquid with a sand mill. After the wet sieve test is qualified, the product is obtained.

[0056] The auxiliary agent includes: 8g propylene glycol (antifreeze agent), 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, and the weight ratio of the magnesium aluminum silicate to the xanthan gum is 10:3:2.

[0058] Comparative Example 1

[0059] A fluazinam and ethiophanate suspension comprises the following components by weight: 10.6% of ethiophanate, 32.1% of fluazinam, 8% of a dispersant, 4.82% of an auxiliary agent, and the balance is made up of deionized water.

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

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

[0062] Step 1, 89.18 g of deionized water, 10 g of Agrilan 755 (comb polymer, Jierun Technology), 6 g of MORWETD-500 (sodium alkylnaphthalene sulfonate, Jierun Technology), and 9.66 g of additives are added to a shearing kettle for shearing and mixed evenly to obtain a mixture;

[0063] Step 2, add 21.23g of ethazolin (Ke Chuang, original drug content 98.9wt%) and 64.26g of fluazinam (Youjia, original drug content 98wt%) into a shearing kettle, shear for 30min, and then grind the uniform shear liquid with a sand mill. After the wet sieve test is qualified, the product is obtained.

[0064] The auxiliary agent includes: 8g propylene glycol (antifreeze agent), 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, and the weight ratio of the magnesium aluminum silicate to the xanthan gum is 10:3:2.

[0066] Comparative Example 2

[0067] A fluazinam and ethiophanate suspension comprises the following components by weight: 10.6% of ethiophanate, 32.1% of fluazinam, 8% of a dispersant, 4.82% of an auxiliary agent, and the balance is made up of deionized water.

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

[0069] A method for preparing a fluazinam and ethazolin suspension 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 (sodium alkylnaphthalene sulfonate formaldehyde condensate, Jierun Technology), and 9.66g of additives into a shearing kettle, shear, mix well, and obtain a mixture;

[0071] Step 2, add 21.23g of ethazolin (Ke Chuang, original drug content 98.9wt%) and 64.26g of fluazinam (Youjia, original drug content 98wt%) into a shearing kettle, shear for 30min, and then grind the uniform shear liquid with a sand mill. After the wet sieve test is qualified, the product is obtained.

[0072] The auxiliary agent includes: 8g propylene glycol (antifreeze agent), 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, and the weight ratio of the magnesium aluminum silicate to the xanthan gum is 10:3:2.

[0074] Comparative Example 3

[0075] A fluazinam and ethiophanate suspension comprises the following components by weight: 10.6% of ethiophanate, 32.1% of fluazinam, 8% of a dispersant, 4.82% of an auxiliary agent, and the balance is made up of deionized water.

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

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

[0078] Step 1, add 89.18g of deionized water, 10g of Agrilan 755 (comb polymer, Jierun Technology), 6g of Agrilan788 (carboxylate dispersant, Jierun Technology) and 9.66g of additives into a shearing kettle, mix well, and obtain a mixture;

[0079] Step 2, add 21.23g of ethazolin (Ke Chuang, original drug content 98.9wt%) and 64.26g of fluazinam (Youjia, original drug content 98wt%) into a shearing kettle, shear for 30min, and then grind the uniform shear liquid with a sand mill. After the wet sieve test is qualified, the product is obtained.

[0080] The auxiliary agent includes: 8g propylene glycol (antifreeze agent), 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, and the weight ratio of the magnesium aluminum silicate to the 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. The test data are listed in Table 1, where “-” indicates that no experiment was conducted.

[0084] 1. Apparent performance of suspension concentrate: at room temperature, observe with naked eyes to see whether there is sanding paste, particles or crystals on screening, crusting, redness of the liquid, etc. If none of the above phenomena occur, it is qualified, otherwise it is unqualified.

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

[0086] 3. Thermal storage performance test: thermal storage at 54℃ for 2 weeks, and then test the apparent performance and D90 particle size.

[0087] Performance test data

[0088] Table 1

[0089]

[0090] like Figure 1 and Figure 2 As shown in Figure 1, the particle size of Example 1 hardly increases after 2 weeks of thermal storage. Figure 3 As shown, after 2 weeks of thermal storage, no particles and crystals were found in the sieve analysis of Example 1, and no wall adhesion was observed. Figure 4-5 As shown, using a dispersant other than the preferred one will cause creaming, particles on sieving, and crusting. Figure 6 As shown, if a preparation method other than the preferred one is used, the liquid will turn red.

Claims

1. A fluazinam and ethazolin suspension, characterized in that: Calculated by weight percentage, the components include: 5-20% of ethidium bromide, 20-40% of fluazinam, 4-15% of dispersant, 1-12% of auxiliary agent, and deionized water to make up the balance.

2. The fluazinam and ethidium cypermethrin suspension according to claim 1, characterized in that The weight ratio of ethidium bromide to fluazinam is 1:(1-5).

3. The fluazinam and ethidium cypermethrin suspension according to claim 2, characterized in that: The dispersant includes at least one of a carboxylate dispersant, a sulfonate dispersant, and a comb polymer.

4. The fluazinam and ethidium cypermethrin suspension according to claim 3, characterized in that: The dispersant comprises a carboxylate dispersant and a comb-like polymer, and the weight ratio of the carboxylate dispersant to the comb-like polymer is 1:(0.2-2).

5. The fluazinam and ethidium cypermethrin suspension according to claim 4, characterized in that: The carboxylate dispersants include polyacid salt dispersants.

6. The fluazinam and ethidium cypermethrin suspension according to claim 5, characterized in that: The comb polymer includes anionic comb polymer.

7. The fluazinam and ethidium cypermethrin suspension according to claim 6, characterized in that: The side chain repeating units of the anionic comb polymer include at least one of ethylene glycol, propylene glycol and butanediol.

8. The fluazinam and ethidium cypermethrin suspension according to claim 7, characterized in that: The auxiliary agent includes at least one of an antifreeze agent, a thickener, a defoaming agent and a preservative, and the thickener includes propylene glycol alginate.

9. A method for preparing the fluazinam and ethidium bromide suspension according to any one of claims 3 to 8, characterized in that: The following steps are involved: Step 1, mixing deionized water, a comb polymer and an additive to obtain a mixture; Step 2, adding ethazofenil and fluazinam to the mixture, mixing evenly, and then adding a carboxylate dispersant, mixing evenly to obtain the product.

10. A use of the fluazinam and ethidium bromide suspension according to any one of claims 1 to 8, characterized in that: Used for the control of mites in cotton, flowers, vegetables and fruit trees.

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