High content suspension concentrate and method of making same

Abstract

The application belongs to the technical field of pesticides, and particularly relates to a high-content suspension agent and a preparation method thereof, the high-content suspension agent comprising, by weight percentage, 50-60% of an active ingredient, 2-6% of a dispersing agent, 6-15% of a wetting agent, 0.2-0.5% of an antifoaming agent, 4-6% of an antifreezing agent, 0.1-2.0% of a thickening agent, and deionized water in the remainder, wherein the application solves the problems of paste formation, flocculation and bottoming in the grinding process of the choline chloride and benzylaminopurine suspension agent by selecting the combination and collocation of various additives, guarantees the stability of the drug, guarantees the control effect of the drug combination, reduces the storage volume, and lowers the cost.

Description

Technical Field

[0001] This invention belongs to the field of pesticide technology, specifically relating to a high-content suspension concentrate and its preparation method. Background Technology

[0002] Suspension concentrates are environmentally friendly, water-based formulations that offer advantages such as safety for operators and users, and relatively low cost. To reduce inventory volume, lower production costs, and minimize packaging and transportation expenses, the production of high-concentration suspension concentrates is increasingly common. Pesticide suspension concentrates are multi-component, heterogeneous, coarsely dispersed systems that exhibit thermodynamic and kinetic instability. In particular, the preparation of high-concentration suspension concentrates presents numerous challenges, including difficulty in milling and paste formation, susceptibility to flocculation, Austronesian ripening, and difficulty in defoaming.

[0003] Choline chloride is a photosynthesis promoter that significantly increases yield and can be used on crops such as wheat, rice, corn, sugarcane, potatoes, vegetables, and grapes. Benzylaminopurine is a synthetic cytokinin with multiple functions, including inhibiting the decomposition of chlorophyll and protein in plant leaves, maintaining green color and preventing aging, and transporting amino acids, auxins, and inorganic salts to the treated parts. It is widely used in agriculture, fruit trees, and horticultural crops. Currently, Shaanxi Meibang has registered a 500g / L benzylaminopurine·choline chloride suspension (4.6+41.4%) with a total content of 45%. However, during the preparation of the choline chloride·benzylaminopurine suspension, issues such as grinding into a paste, excessive bubbles, large particle size, and flocculation occur during grinding. Furthermore, it easily clumps during hot storage, resulting in an unstable preparation.

[0004] The key to ensuring the efficacy of choline chloride-benzylaminopurine suspension lies in its ability to prepare high-content suspensions, address issues such as paste formation and flocculation during the grinding process, and maintain the stability of the suspensions. This is crucial for maximizing drug efficacy. Furthermore, high-content suspensions can reduce inventory volume, lower production costs, and reduce packaging and transportation expenses. Summary of the Invention

[0005] Based on the above, this invention provides a high-content suspension and its preparation method. By selecting a combination of various adjuvants, the problems of viscous paste formation and flocculation at the bottom during the grinding process of choline chloride·benzylaminopurine suspension are solved, ensuring the stability of the drug and thus ensuring the prevention and treatment effect of the drug combination. At the same time, the storage volume is reduced, and transportation and packaging costs are lowered.

[0006] The technical solution of the present invention is as follows:

[0007] A high-content suspending agent, the active ingredients of which are choline chloride and benzylaminopurine, comprises, by weight percentage, 50-60% active ingredients, 2-6% dispersant, 6-15% wetting agent, 0.2%-0.5% defoamer, 4%-6% antifreeze agent, 0.1%-2.0% thickener, and the balance being deionized water.

[0008] Preferably, the weight ratio of choline chloride to benzylaminopurine in the active ingredient is 6-9:1.

[0009] Preferably, the dispersant is one or more of the following: a polymeric amphiphilic anionic nonionic surfactant, a comb-shaped polycarboxylate dispersant, an alkyl naphthalene sulfonate formaldehyde condensate, a modified carboxylate copolymer, and a carboxylic acid dispersant.

[0010] Among them are amphiphilic anionic surfactants such as SP-SC29 (Jiangsu Qingyu Chemical Technology Co., Ltd.), comb-structured polycarboxylate dispersants such as SP-27001 (Jiangsu Qingyu Chemical Technology Co., Ltd.), alkyl naphthalene sulfonate formaldehyde condensates such as Morwet D-425 (Nanjing Jierun Technology Co., Ltd.), modified carboxylate copolymers such as Agrilan 788 (Nanjing Jierun Technology Co., Ltd.), and carboxylic acid dispersants such as GY-D07 (Beijing Guangyuan Yinong Chemical Co., Ltd.).

[0011] More preferably, the dispersant is one or two of the following: a polymeric amphiphilic anionic nonionic surfactant and a comb-structured polycarboxylate dispersant.

[0012] More preferably, the dispersant is a polymeric amphiphilic anionic nonionic surfactant SP-SC29 and a polycarboxylate dispersant SP-27001.

[0013] Preferably, the wetting agent is one or more of low-foaming wetting agents and fatty alcohol polyoxyethylene ethers.

[0014] Among them, at least one of the following is a low-foaming wetting agent: GY-W07 (Beijing Guangyuan Yinong Chemical Co., Ltd.) or fatty alcohol polyoxyethylene ether;

[0015] More preferably, the wetting agent is fatty alcohol polyoxyethylene ether with a degree of polymerization n = 5-9.

[0016] Preferably, the defoamer is a trisiloxane-based defoamer.

[0017] Preferably, the thickener is one or both of xanthan gum and silica.

[0018] Preferably, the antifreeze is one or both of glycerol and ethylene glycol.

[0019] A method for preparing a high-content suspending agent, the specific preparation steps are as follows:

[0020] 1) First, mix deionized water and choline chloride technical material to completely dissolve choline chloride, then add wetting agent, dispersant, thickener, defoamer, antifreeze agent and benzylaminopurine technical material, and stir evenly;

[0021] 2) Add the mixture from step (1) to a sand mill for grinding until the particle size D95 = 5 μm. During the grinding process, the temperature is controlled below 30℃. After grinding, choline chloride·benzylaminopurine suspension is obtained.

[0022] In the existing technology for preparing choline chloride·benzylaminopurine suspension, problems such as paste formation during grinding, excessive bubbles, large particle size, flocculation, and easy crusting during heat storage are encountered. The inventors believe these problems are related to choline chloride, which is highly water-soluble and easily traps water molecules, making grinding difficult and leading to flocculation and paste formation. Through continuous exploration, the inventors discovered that by combining different functional adjuvants, the binding of choline chloride to water molecules is released, solving the problems of viscous paste formation and flocculation during the grinding process of choline chloride·benzylaminopurine suspension, thus ensuring the preventive and therapeutic effects of the drug. This invention utilizes a combination of a high-molecular-weight amphiphilic anionic nonionic surfactant, a comb-structured polycarboxylate dispersant, and a fatty alcohol polyoxyethylene ether. The fatty alcohol polyoxyethylene ether effectively binds to water-soluble choline chloride, preventing choline chloride from binding water molecules and causing high viscosity and paste-like formation during grinding. Simultaneously, the combination of the high-molecular-weight amphiphilic anionic nonionic surfactant and the comb-structured polycarboxylate dispersant increases the double-layer thickness of the particle surface and reduces the steric hindrance of the macromolecular chains, solving the flocculation problem of the suspension and making the formulation more stable. In this invention, choline chloride and benzylaminopurine, combined with specific adjuvants, ultimately produce a high-content suspension with both high active ingredient content and excellent stability and suspension rate.

[0023] This invention provides a high-content suspension concentrate and its preparation method. By selecting and combining multiple functional adjuvants, it solves the problems of paste formation and flocculation during the grinding process of choline chloride·benzylaminopurine suspension concentrate, ensuring the stability and suspension rate of the drug, thereby guaranteeing the prevention and control effect of the drug combination. At the same time, it reduces the storage volume and lowers costs. The prepared choline chloride·benzylaminopurine suspension concentrate is a water-based environmentally friendly preparation, which is beneficial to the protection of the agricultural ecological environment. In this invention, the choline chloride·benzylaminopurine suspension concentrate has a high content of active ingredients, which can reduce the storage volume, reduce production costs, and reduce packaging and transportation costs. Attached Figure Description

[0024] Figure 1 This is a microscopic observation of the sample in Comparative Example 1 after it has been diluted with water.

[0025] Figure 2This is a microscopic observation of the sample in Example 1 after it has been diluted with water.

[0026] Figure 3 This is a diagram showing the paste-like state that appeared during the preparation process in Comparative Example 4;

[0027] In the figure, the sample of Example 1 diluted with water was observed under a microscope, and the drug particle size distribution was uniform. The sample of Comparative Example 1 diluted with water was observed under a microscope, and the drug particles were flocculated. Detailed Implementation

[0028] The technical solutions in the embodiments of the present invention will be clearly and completely described below. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0029] Unless otherwise specified, the experimental methods used in the following examples are conventional methods.

[0030] SP-SC29 was purchased from Jiangsu Qingyu Chemical Technology Co., Ltd.; SP-27001 was purchased from Jiangsu Qingyu Chemical Technology Co., Ltd.; Morwet D-425 was purchased from Nanjing Jierun Technology Co., Ltd.; Agrilan 788 was purchased from Nanjing Jierun Technology Co., Ltd.; GY-D07 and GY-W07 were purchased from Beijing Guangyuan Yinong Chemical Co., Ltd.

[0031] Unless otherwise specified, all raw materials and reagents used in the following examples and comparative examples are commercially available.

[0032] Example 1: 50% choline chloride·benzylaminopurine suspension

[0033] Choline chloride technical grade, 45%; benzylaminopurine technical grade, 5%; SP-SC29, 2%; SP-27001, 2%; fatty alcohol polyoxyethylene ether AEO-5, 12%; Sag 1522, 0.2%; ethylene glycol, 4%; xanthan gum, 0.1%; silica, 1%; deionized water, to make up to 100%.

[0034] Example 2: 50% choline chloride·benzylaminopurine suspension

[0035] Choline chloride technical grade, 45%; benzylaminopurine technical grade, 5%; SP-SC29, 2%; SP-27001, 3%; fatty alcohol polyoxyethylene ether AEO-7, 10%; Sag 1522, 0.2%; ethylene glycol, 4%; xanthan gum, 0.1%; silica, 1%; deionized water, to make up to 100%.

[0036] Example 3: 50% choline chloride·benzylaminopurine suspension

[0037] Choline chloride technical grade, 45%; benzylaminopurine technical grade, 5%; SP-SC29, 3%; SP-27001, 1%; fatty alcohol polyoxyethylene ether AEO-9, 8%; Sag 1522, 0.2%; ethylene glycol, 4%; xanthan gum, 0.1%; silica, 1%; deionized water, to make up to 100%.

[0038] Comparative Example 1: 50% Choline Chloride·Benzylaminopurine Suspension

[0039] Choline chloride technical grade, 45%; benzylaminopurine technical grade, 5%; SP-SC29, 2%; SP-27001, 2%; GY-W07, 12%; Sag 1522, 0.2%; ethylene glycol, 4%; xanthan gum, 0.1%; silica, 1%; deionized water, to make up to 100%.

[0040] Compared with Example 1, in Comparative Example 1, the wetting agent fatty alcohol polyoxyethylene ether AEO-5 was replaced with GY-W07.

[0041] Comparative Example 2: 50% Choline Chloride·Benzylaminopurine Suspension

[0042] Choline chloride technical grade, 45%; benzylaminopurine technical grade, 5%; SP-SC29, 2%; GY-D07, 2%; fatty alcohol polyoxyethylene ether AEO-5, 12%; Sag 1522, 0.2%; ethylene glycol, 4%; xanthan gum, 0.1%; silica, 1%; deionized water, to make up to 100%.

[0043] Compared with Example 1, in Comparative Example 2, the dispersant SP-27001 was replaced with GY-D07.

[0044] Comparative Example 3: 50% Choline Chloride·Benzylaminopurine Suspension

[0045] Choline chloride technical grade, 45%; benzylaminopurine technical grade, 5%; Morwet D-425, 2%; SP-27001, 2%; fatty alcohol polyoxyethylene ether AEO-5, 12%; Sag 1522, 0.2%; ethylene glycol, 4%; xanthan gum, 0.1%; silica, 1%; deionized water, to make up to 100%.

[0046] Compared with Example 1, in Comparative Example 3, the dispersant SP-SC29 was replaced with Morwet D-425.

[0047] Comparative Example 4: 50% Choline Chloride·Benzylaminopurine Suspension

[0048] Choline chloride technical grade, 45%; benzylaminopurine technical grade, 5%; Morwet D-425, 2%; Agrilan 788, 2%; GY-W07, 12%; Sag 1522, 0.2%; ethylene glycol, 4%; xanthan gum, 0.1%; silica, 1%; deionized water, to make up to 100%.

[0049] Compared with Example 1, in Comparative Example 4, the dispersant SP-SC29 was replaced with Morwet D-425, SP-27001 was replaced with Agrilan 788, and the wetting agent fatty alcohol polyoxyethylene ether AEO-5 was replaced with GY-W07.

[0050] The above-mentioned choline chloride·benzylaminopurine suspension was prepared by the following steps: First, deionized water and choline chloride technical were mixed to completely dissolve choline chloride. Then, wetting agent, dispersant, thickener, defoamer, antifreeze agent and benzylaminopurine technical were added and stirred evenly. 2) The mixture in step (1) was added to a sand mill for grinding until the particle size D95 = 5 μm. The temperature was controlled below 30°C during the grinding process. After grinding, the choline chloride·benzylaminopurine suspension was obtained.

[0051] Test case

[0052] The following methods were used for testing: 1. Mass fraction of active ingredient: The mass fraction of benzylaminopurine was determined by high performance liquid chromatography (HPLC); the mass fraction of choline chloride was determined by ion chromatography (IGC). 2. Determination of suspension rate of active ingredient: The suspension rate was determined according to "Method 2" in GB / T 14825. 3. Thermal storage stability of pesticides: The samples were stored at (54±2)℃ for 14 days, mainly testing the content of active ingredient, suspension rate, and particle size. 4. Freeze-thaw stability: The samples were subjected to freeze-thaw stability tests. The freezing and thawing stability tests were performed in four cycles between (-10±2)℃ and (20±2)℃, with each cycle freezing for 18 hours and thawing for 6 hours. The main tests were testing the content of active ingredient, suspension rate, and particle size. 5. During and after grinding, the samples were diluted with water and observed under a microscope for flocculation. Examples 1-3 and Comparative Examples 1-3 were subjected to thermal storage and freeze-thaw experiments. The specific data are shown in the table below: (A is choline chloride, B is benzylaminopurine)

[0053]

[0054]

[0055] As shown in the table above, the grinding state and microscopic particle size distribution of the samples in Examples 1-3 were relatively uniform. After heat storage and freeze-thaw cycles, the samples in Examples 1-3 showed little difference from the samples at room temperature, indicating good sample stability. Comparative Examples 1-3, compared to the Examples, only replaced one of the additives, resulting in a decrease in the suspension rate of the active ingredient and an increase in particle size. After heat storage and freeze-thaw cycles, the samples in Comparative Examples 1-3 showed a significant difference from the samples at room temperature, indicating poor sample stability and flocculation observed under a microscope. Comparative Example 4, compared to the Examples, replaced both the dispersant and wetting agent, resulting in a significant decrease in the suspension rate of its active ingredient and a significant increase in particle size. During the grinding process, the sample became paste-like. Figure 3 As shown, microscopic observation revealed severe flocculation. Comparison shows that the combination of the amphiphilic anionic nonionic surfactant SP-SC29, the polycarboxylate dispersant SP-27001, and fatty alcohol polyoxyethylene ethers (n=5-9) can yield a stable choline chloride·benzylaminopurine suspension.

[0056] This invention provides a high-content suspension concentrate and its preparation method. By selecting and combining functional adjuvants, the method solves the problems of paste formation and flocculation during the grinding process of choline chloride·benzylaminopurine suspension concentrate, ensuring the stability and suspension rate of the drug, thereby guaranteeing the prevention and control effect of the drug combination. At the same time, it reduces the storage volume and lowers costs. The prepared choline chloride·benzylaminopurine suspension concentrate is a water-based environmentally friendly preparation, which is beneficial to the protection of the agricultural ecological environment. Due to its high content of active ingredients, the choline chloride·benzylaminopurine suspension concentrate of this invention can reduce the storage volume, production costs, packaging, and transportation costs.

Claims

1. A high-content suspending agent, characterized in that, Its active ingredients are choline chloride and benzylaminopurine. By weight percentage, this high-content suspension includes: choline chloride technical grade, 45%; benzylaminopurine technical grade, 5%; SP-SC29, 2%; SP-27001, 2%; fatty alcohol polyoxyethylene ether AEO-5, 12%; Sag 1522, 0.2%; ethylene glycol, 4%; xanthan gum, 0.1%; silica, 1%; deionized water, to make up to 100%. Alternatively, it may include: choline chloride technical grade, 45%; benzylaminopurine technical grade, 5%; SP-SC29, 2%; SP-27001, 3%; fatty alcohol polyoxyethylene ether AEO-7, 10%; Sag 1522, 0.2%; ethylene glycol, 4%; xanthan gum, 0.1%; silica, 1%; deionized water, to make up to 100%. Alternatively, it may include: choline chloride technical grade, 45%; benzylaminopurine technical grade, 5%; SP-SC29, 3%; SP-27001, 1%; fatty alcohol polyoxyethylene ether AEO-9, 8%; Sag 1522, 0.2%; ethylene glycol, 4%; xanthan gum, 0.1%; silica, 1%; and deionized water to make up to 100%.

2. The method for preparing a high-content suspending agent according to claim 1, characterized in that, The specific preparation steps are as follows: 1) First, mix deionized water and choline chloride raw material to completely dissolve choline chloride. Then add fatty alcohol polyoxyethylene ether, SP-SC29, SP-27001, xanthan gum, silica, Sag 1522, ethylene glycol, and benzylaminopurine raw material, and stir well. 2) Add the mixture from step (1) to a sand mill for grinding until the particle size D95 = 5 μm. During the grinding process, the temperature is controlled below 30℃. After grinding, choline chloride·benzylaminopurine suspension is obtained.

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