A high-stability pyraclostrobin suspension concentrate and a preparation method thereof
By using trifluoride containing hydroxyl groups as a dispersant, the composition and preparation process of pyraclostrobin suspension were optimized, solving the stability problem of nanoscale suspensions and achieving a pyraclostrobin suspension with high stability and good efficacy.
Patent Information
- Application Number
- CN202411821688.X
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2024-12-11
- Publication Date
- 2025-12-19
- Estimated Expiration
- 2044-12-11
AI Technical Summary
The poor stability of nano-sized pyraclostrobin suspension affects the efficacy of the drug.
A suspending agent was prepared by using trifluorides containing hydroxyl groups as dispersants, particularly the combination of 2,2,2-trifluoroethanol and 4-(trifluoromethyl)benzyl alcohol, with an optimized ratio of 1:9 to 9:1, and combining them with wetting agents, thickeners, antifreeze agents and defoamers through a sand milling process.
The thermal stability of pyraclostrobin suspension was improved, and the suspension rate remained at around 95% after heat storage, avoiding crystallization and paste formation, and significantly improving the stability of the agent.
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Abstract
Description
TECHNICAL FIELD
[0001] The present application relates to the technical field of pesticides, in particular to a high-stability pyraclostrobin suspension agent and a preparation method thereof. BACKGROUND
[0002] Pyraclostrobin is a methoxy acrylate fungicide, which has a wider fungicidal spectrum and higher fungicidal activity, and has the effects of protection, treatment and eradication, such as: ① improving crop quality, increasing chlorophyll content, enhancing photosynthesis and carbohydrate accumulation; ② improving the stress resistance of crops; ③ improving the fruit setting rate; ④ acting quickly and having a long effective period. Due to the above advantages, it is often used as a pesticide.
[0003] The pesticide dosage form can be selected from environmentally friendly dosage forms such as suspension agent, microcapsule suspension agent, water agent, emulsion in water, microemulsion, granule, water dispersible granule and soluble granule, and the suspension agent is the most commonly used pesticide dosage form.
[0004] In the field of pesticides, the smaller the particle size of the suspension agent, the better the effect of the pesticide, so the development of nanoscale suspension agents has generally begun. However, although the nanoscale suspension agent has good efficacy, it generally has the problem of poor stability. SUMMARY
[0005] The present application provides a high-stability pyraclostrobin suspension agent and a preparation method thereof, which solves the problem of poor stability of the nanoscale pyraclostrobin suspension agent with good efficacy in the related art.
[0006] The technical scheme of the present application is as follows:
[0007] A high-stability pyraclostrobin suspension agent, the raw materials of which include pyraclostrobin, a dispersing agent, a wetting agent, a thickening agent and water, and the dispersing agent is a trifluoride containing a hydroxyl group.
[0008] The trifluoride containing a hydroxyl group in the present application can be any compound containing a hydroxyl group and three fluorine atoms connected to the same carbon.
[0009] As a further technical scheme, the raw materials further include an antifreeze agent and a defoaming agent.
[0010] As a further technical scheme, the raw materials are composed of the following components in mass percentage: pyraclostrobin 25% to 30%, dispersing agent 5% to 10%, wetting agent 1% to 3%, thickening agent 0.4% to 0.8%, antifreeze agent 1% to 5%, defoaming agent 0.1% to 0.3%, and the balance of water.
[0011] As a further technical scheme, the dispersing agent includes 2,2,2-trifluoroethanol and / or 4-(trifluoromethyl)benzyl alcohol.
[0012] As a further technical solution, the dispersant is composed of 2,2,2-trifluoroethanol and 4-(trifluoromethyl) benzyl alcohol in a ratio of 1:9 to 9:1 in terms of mass percentage.
[0013] The present application optimizes the dispersant to be 2,2,2-trifluoroethanol and 4-(trifluoromethyl) benzyl alcohol in a mass ratio of 1:9 to 9:1, further improving the thermal stability of the pyraclostrobin suspension concentrate.
[0014] As a further technical solution, the amount of 2,2,2-trifluoroethanol is ≤ the amount of 4-(trifluoromethyl) benzyl alcohol in terms of mass percentage.
[0015] The present application limits the mass of 2,2,2-trifluoroethanol to be ≤ the mass of 4-(trifluoromethyl) benzyl alcohol, further improving the thermal stability of the pyraclostrobin suspension concentrate.
[0016] As a further technical solution, the dispersant is composed of 2,2,2-trifluoroethanol and 4-(trifluoromethyl) benzyl alcohol in a ratio of 7:3 in terms of mass percentage.
[0017] The present application limits 2,2,2-trifluoroethanol and 4-(trifluoromethyl) benzyl alcohol in a mass ratio of 7:3 as a dispersant, further improving the thermal stability of the pyraclostrobin suspension concentrate.
[0018] As a further technical solution, the wetting agent includes one or both of alkyl naphthalene sulfonate and alkyl phenol polyoxyethylene ether.
[0019] The thickening agent includes one or both of xanthan gum and magnesium aluminum silicate.
[0020] As a further technical solution, the antifreeze agent includes one or more of ethylene glycol, propylene glycol, and glycerol.
[0021] The defoaming agent is an organic silicon defoaming agent.
[0022] The present application also proposes a preparation method of a high-stability pyraclostrobin suspension concentrate, including the following steps: uniformly mixing raw materials, sand milling, and obtaining the pyraclostrobin suspension concentrate.
[0023] As a further technical solution, the mixing time is 60 to 90 min.
[0024] The working principle and beneficial effects of the present application are as follows:
[0025] The present application provides a pyraclostrobin suspension agent with good stability, which is prepared by pyraclostrobin, a dispersing agent containing trifluoride with hydroxyl, a wetting agent, a thickening agent and water as part of raw materials. The prepared pyraclostrobin suspension agent can be nanoscale, has good efficacy and good thermal stability, and the suspension rate is about 95% before and after thermal storage, and the fluidity is normal after processing and thermal storage, without crystallization and creaming. Compared with the traditional dispersing agent, the dispersing agent containing trifluoride with hydroxyl has better effect, and can improve the thermal stability of the pyraclostrobin suspension agent. DETAILED DESCRIPTION
[0026] The technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the embodiments of the present application. Obviously, the described embodiments are only part of the embodiments of the present application, rather than all the embodiments. Based on the embodiments in the present application, all other embodiments obtained by those skilled in the art without creative labor are within the scope of protection of the present application.
[0027] The parameters of the raw materials in the following examples and comparative examples are as follows:
[0028] The alkyl naphthalene sulfonate is Petro 22N sodium alkyl naphthalene sulfonate;
[0029] The alkyl phenol polyoxyethylene ether is nonyl phenol polyoxyethylene ether;
[0030] The defoaming agent is Momentive SAG 1572 silicone defoaming agent.
[0031] Example 1
[0032] According to the mass percentage, pyraclostrobin 30%, 4-(trifluoromethyl) benzyl alcohol 10%, alkyl naphthalene sulfonate 3%, xanthan gum 0.3%, magnesium aluminum silicate 0.5%, propylene glycol 5%, defoaming agent 0.3% and the balance of water are mixed, and then homogenously dispersed at 1500 rpm for 90 min, and then sand ground to obtain a pyraclostrobin suspension agent.
[0033] Example 2
[0034] According to the mass percentage, pyraclostrobin 25%, 4-(trifluoromethyl) benzyl alcohol 5%, alkyl phenol polyoxyethylene ether 1%, xanthan gum 0.4%, ethylene glycol 1%, defoaming agent 0.1% and the balance of water are mixed, and then homogenously dispersed at 1500 rpm for 60 min, and then sand ground to obtain a pyraclostrobin suspension agent.
[0035] Example 3
[0036] Pyraclostrobin 30%, 2,2,2-trifluoroethanol 10%, alkyl naphthalene sulfonate 3%, xanthan gum 0.3%, magnesium aluminum silicate 0.5%, propylene glycol 5%, antifoaming agent 0.3% and the balance of water were mixed according to mass percentage, and after homogenously dispersing for 90 min at 1500 rpm, sand grinding was performed to obtain pyraclostrobin suspension concentrate.
[0037] Example 4
[0038] Pyraclostrobin 30%, 2,2,2-trifluoroethanol 9%, 4-(trifluoromethyl)benzyl alcohol 1%, alkyl naphthalene sulfonate 3%, xanthan gum 0.3%, magnesium aluminum silicate 0.5%, propylene glycol 5%, antifoaming agent 0.3% and the balance of water were mixed according to mass percentage, and after homogenously dispersing for 90 min at 1500 rpm, sand grinding was performed to obtain pyraclostrobin suspension concentrate.
[0039] Example 5
[0040] Pyraclostrobin 30%, 2,2,2-trifluoroethanol 5%, 4-(trifluoromethyl)benzyl alcohol 5%, alkyl naphthalene sulfonate 3%, xanthan gum 0.3%, magnesium aluminum silicate 0.5%, propylene glycol 5%, antifoaming agent 0.3% and the balance of water were mixed according to mass percentage, and after homogenously dispersing for 90 min at 1500 rpm, sand grinding was performed to obtain pyraclostrobin suspension concentrate.
[0041] Example 6
[0042] Pyraclostrobin 30%, 2,2,2-trifluoroethanol 3%, 4-(trifluoromethyl)benzyl alcohol 7%, alkyl naphthalene sulfonate 3%, xanthan gum 0.3%, magnesium aluminum silicate 0.5%, propylene glycol 5%, antifoaming agent 0.3% and the balance of water were mixed according to mass percentage, and after homogenously dispersing for 90 min at 1500 rpm, sand grinding was performed to obtain pyraclostrobin suspension concentrate.
[0043] Example 7
[0044] Pyraclostrobin 30%, 2,2,2-trifluoroethanol 1%, 4-(trifluoromethyl)benzyl alcohol 9%, alkyl naphthalene sulfonate 3%, xanthan gum 0.3%, magnesium aluminum silicate 0.5%, propylene glycol 5%, antifoaming agent 0.3% and the balance of water were mixed according to mass percentage, and after homogenously dispersing for 90 min at 1500 rpm, sand grinding was performed to obtain pyraclostrobin suspension concentrate.
[0045] Comparative Example 1
[0046] Pyraclostrobin 30%, British Tensol 7500 carboxylate dispersant 10%, alkyl naphthalene sulfonate 3%, xanthan gum 0.3%, magnesium aluminum silicate 0.5%, propylene glycol 5%, antifoaming agent 0.3% and the balance of water were mixed according to mass percentage, and after homogenously dispersing for 90 min at 1500 rpm, sand grinding was performed to obtain pyraclostrobin suspension concentrate.
[0047] The pyraclostrobin suspensions obtained in Examples 1-7 and Comparative Example 1 were subjected to initial particle size D98 and particle size D98 tests after storage at 54±2℃ for 14 days, according to the method in GB T 19136-2021, and the change rate was calculated according to the following formula:
[0048] Change rate (%) = (particle size D98 after storage at 54±2℃ for 14 days - initial particle size D98) ÷ initial particle size D98 x 100;
[0049] The test results are recorded in Table 1.
[0050] Table 1 Thermal stability of pyraclostrobin suspension
[0051]
[0052] As can be seen from Table 1, the pyraclostrobin suspension provided by the present application has good thermal stability.
[0053] Compared with Comparative Example 1, the pyraclostrobin suspension obtained by adding a trifluoride containing hydroxyl group as a dispersant in Examples 1-7 has a lower change rate after thermal storage, indicating that compared with traditional dispersants, the trifluoride containing hydroxyl group as a dispersant has better effect and can improve the thermal stability of the pyraclostrobin suspension.
[0054] The pyraclostrobin suspension obtained in Examples 4-7 has a lower change rate after thermal storage than that in Examples 1 and 3, indicating that the dispersant is 2,2,2-trifluoroethanol and 4-(trifluoromethyl)benzyl alcohol in a mass ratio of 1:9-9:1, which can further improve the thermal stability of the pyraclostrobin suspension.
[0055] The pyraclostrobin suspension obtained in Examples 5-7 has a lower change rate after thermal storage than that in Example 4, indicating that the mass of 2,2,2-trifluoroethanol is ≤ the mass of 4-(trifluoromethyl)benzyl alcohol, which can further improve the thermal stability of the pyraclostrobin suspension.
[0056] The pyraclostrobin suspension obtained in Example 6 has a lower change rate after thermal storage than that in Examples 5 and 7, indicating that the mass ratio of 2,2,2-trifluoroethanol and 4-(trifluoromethyl)benzyl alcohol is 7:3, which can further improve the thermal stability of the pyraclostrobin suspension.
[0057] The above is only a preferred embodiment of the present application and is not intended to limit the present application. Any modification, equivalent replacement, improvement, etc. made within the spirit and principles of the present application shall be included in the protection scope of the present application.
Claims
1. A suspension of pyraclostrobin, characterized in that, The raw material is composed of the following components in mass percentage: 25-30% of pyraclostrobin, 5-10% of dispersing agent, 1-3% of wetting agent, 0.4-0.8% of thickening agent, 1-5% of antifreezing agent, 0.1-0.3% of defoaming agent and the balance of water; the dispersing agent is composed of 2,2,2-trifluoroethanol and 4-(trifluoromethyl)benzyl alcohol in a weight ratio of 1:9-9:1; the wetting agent is alkyl naphthalene sulfonate or alkyl phenol polyoxyethylene ether; the thickening agent comprises one or both of xanthan gum and magnesium aluminum silicate; the antifreezing agent is ethylene glycol, propylene glycol or glycerol; and the defoaming agent is a silicone defoaming agent.
2. The pyraclostrobin suspension agent according to claim 1, characterized in that, The amount of 2,2,2-trifluoroethanol is ≤ the amount of 4-(trifluoromethyl)benzyl alcohol in mass percentage.
3. The pyraclostrobin suspension agent according to claim 2, characterized in that, The dispersing agent is composed of 2,2,2-trifluoroethanol and 4-(trifluoromethyl)benzyl alcohol in a ratio of 7:3 in mass percentage.
4. The preparation method of the fluoxastrobin suspending agent according to any one of claims 1-3, characterized in that, The method comprises the following steps: After the raw material is uniformly mixed, sanding is performed to obtain pyraclostrobin suspension concentrate. After the raw material is uniformly mixed, sanding is performed to obtain pyraclostrobin suspension concentrate.
Citation Information
Patent Citations
Pyraclostrobin suspension concentrate and preparation method thereof
CN111184013A
Pyraclostrobin-containing suspending agent as well as preparation process and application thereof
CN116491518A