Pyriproxyfen-containing soluble concentrate and preparation method thereof

Abstract

The invention relates to the technical field of pesticides, and discloses a pyriproxyfen-containing soluble concentrate and a preparation method thereof. The pyriproxyfen-containing soluble concentrate provided by the invention is prepared from the following components in parts by weight: 1 to 10 parts of pyriproxyfen active compound, 70 to 80 parts of dichlorvos active compound, 10 to 20 parts of emulsifier and 1 to 5 parts of stabilizer. According to the pyriproxyfen-containing soluble concentrate provided by the invention, the nerve poison dichlorvos and the insect growth regulator pyriproxyfen are combined to form a prevention and control system covering the whole life cycle of pests, and the emulsifier and the stabilizer are matched, so that the soluble concentrate has relatively good content stability under the conditions of normal temperature and heat storage, and the decomposition rate of effective components is reduced.

Description

Technical Field

[0001] This invention relates to the field of pesticide technology, specifically to a soluble agent containing pyriproxyfen and its preparation method. Background Technology

[0002] Pyriproxyfen is an insect growth regulator that disrupts the normal growth of insects. It is a novel insecticide belonging to the juvenile hormone analogue family, and its inhibitory effect on insects is mainly manifested in affecting molting and reproduction. It possesses systemic translocation activity, a long residual effect, crop safety, and minimal impact on the ecological environment. Furthermore, pyriproxyfen has good control effects on pear psyllids, whiteflies, scale insects, diamondback moths, beet armyworms, cotton bollworms, citrus psyllids, thrips, and rice stem borers.

[0003] Dichlorvos (chemical name: O,O-dimethyl-O-(2,2-dichlorovinyl)phosphate) is a broad-spectrum, highly effective, and fast-acting organophosphorus insecticide and acaricide. Currently, it is mainly used in limited areas such as pest control on crops like rice, wheat, corn, cotton, cruciferous vegetables, cucumbers, and apples, as well as for sanitary pest control (such as mosquitoes and flies) and pest control in storage facilities.

[0004] However, existing technologies have significant drawbacks in the combined use of pyriproxyfen and dichlorvos. Because dichlorvos is highly hydrolyzable and acidic (pH 1.5-4.0), and pyriproxyfen is prone to intramolecular cyclization degradation under acidic conditions, direct combination in traditional formulations leads to pyriproxyfen decomposition. Attempts to address this issue have focused on improving the combination system, but often at the cost of reducing dichlorvos content and sacrificing its activity, failing to achieve perfect compatibility between the two. Therefore, developing a combination scheme that maintains pyriproxyfen stability without affecting dichlorvos content has become an urgent problem to solve. Summary of the Invention

[0005] This invention provides a soluble agent containing pyriproxyfen and its preparation method to solve the problem that the combination of pyriproxyfen and dichlorvos leads to the decomposition of pyriproxyfen or a reduction in the content of dichlorvos.

[0006] In a first aspect, the present invention provides a soluble concentrate containing pyriproxyfen, comprising, by weight: 1-10 parts of pyriproxyfen technical, 70-80 parts of dichlorvos technical, 10-20 parts of emulsifier, and 1-5 parts of stabilizer.

[0007] In one alternative embodiment, the emulsifier comprises at least one of ammonium dodecylbenzenesulfonate, polyoxyethylene castor oil, and styrene-phenol polyoxyethylene ether.

[0008] In one alternative embodiment, the stabilizer includes at least one of butylated hydroxytoluene, tert-butylhydroquinone, and butylated hydroxyanisole.

[0009] In one optional embodiment, the mixture comprises, by weight: 10 parts of pyriproxyfen technical, 70 parts of dichlorvos technical, 15 parts of emulsifier, and 5 parts of stabilizer, wherein the emulsifier is polyoxyethylene castor oil and ammonium dodecylbenzenesulfonate in a mass ratio of 1-2:1, and the stabilizer is butylated hydroxytoluene.

[0010] In one optional embodiment, the mixture comprises, by weight: 5.1 parts of pyriproxyfen technical, 78.9 parts of dichlorvos technical, 14 parts of emulsifier, and 2 parts of stabilizer, wherein the emulsifier is styrene-phenol polyoxyethylene ether and polyoxyethylene castor oil in a mass ratio of 1:1-2, and the stabilizer is butylated hydroxytoluene.

[0011] In one optional embodiment, the mixture comprises, by weight: 1 part pyriproxyfen technical, 80 parts dichlorvos technical, 18 parts emulsifier, and 1 part stabilizer, wherein the emulsifier is styrene-phenol polyoxyethylene ether and ammonium dodecylbenzenesulfonate in a mass ratio of 1-2:1, and the stabilizer is butylated hydroxytoluene.

[0012] In one optional embodiment, the pyriproxyfen technical material contains ≥98% pyriproxyfen.

[0013] In one optional embodiment, the dichlorvos technical material contains ≥95% dichlorvos.

[0014] Secondly, the present invention provides a method for preparing the above-mentioned pyriproxyfen-containing soluble concentrate, comprising the following steps: mixing pyriproxyfen technical material and dichlorvos technical material, adding emulsifier and stabilizer for emulsification, and obtaining a pyriproxyfen-containing soluble concentrate.

[0015] In one optional embodiment, the mixing speed is 300-500 rpm and the time is 10-30 min.

[0016] In one optional embodiment, the emulsification rotation speed is 300-500 rpm and the time is 10-30 min.

[0017] The technical solution of this invention has the following advantages:

[0018] 1. This invention provides a soluble concentrate containing pyriproxyfen, comprising, by weight: 1-10 parts pyriproxyfen technical, 70-80 parts dichlorvos technical, 10-20 parts emulsifier, and 1-5 parts stabilizer. Soluble concentrates (SL), as an important formulation of modern pesticides, have significant advantages over traditional formulations (such as emulsifiable concentrates (EC), wettable powders (WP), and powders (DP),) especially in terms of environmental friendliness, safety, ease of use, and efficacy stability. They can fundamentally solve the solvent pollution problem of traditional pesticides while improving application efficiency and safety. The soluble concentrate containing pyriproxyfen provided by this invention combines the neurotoxin dichlorvos with the insect growth regulator pyriproxyfen to form a control system covering the entire life cycle of pests. Dichlorvos exerts a rapid killing effect on adult insects, knocking down mosquitoes, flies, cockroaches, and other sanitary pests within minutes of contact. Pyriproxyfen inhibits chitin synthesis in larvae, blocking the development of eggs and pupae, thus cutting off the reproductive chain at its source. Furthermore, the soluble concentrate is combined with emulsifiers and stabilizers, giving it good content stability under normal temperature and heat storage conditions. This allows for maintaining a high content of dichlorvos while reducing the decomposition rate of pyriproxyfen, resulting in a final soluble concentrate with good activity.

[0019] 2. This invention provides a soluble concentrate containing pyriproxyfen, comprising, by weight: 5.1 parts pyriproxyfen technical, 78.9 parts dichlorvos technical, 14 parts emulsifier, and 2 parts stabilizer. The emulsifier is a mixture of styrene-phenol polyoxyethylene ether and polyoxyethylene castor oil in a mass ratio of 1:1-2, and the stabilizer is butylated hydroxytoluene. This invention employs a specific combination of emulsifiers and a specific stabilizer to achieve a synergistic effect, resulting in good stability of the content of the active ingredients pyriproxyfen and dichlorvos in the soluble concentrate, thus ensuring good activity.

[0020] 3. This invention provides a method for preparing a pyriproxyfen-containing soluble concentrate, comprising the following steps: mixing pyriproxyfen technical and dichlorvos technical, adding an emulsifier and a stabilizer for emulsification, to obtain a pyriproxyfen-containing soluble concentrate. This preparation method represents a breakthrough in the integration of pesticide compounding technology and environmentally friendly formulations. By preparing two pesticides with different insecticidal mechanisms into a soluble concentrate, it achieves a balance between high-efficiency insecticidal activity, environmental friendliness, and operational safety. Detailed Implementation

[0021] The following embodiments are provided to better understand the present invention, but the following embodiments do not constitute a limitation on the content and scope of protection of the present invention. Any product that is the same as or similar to the present invention, derived by any person under the guidance of the present invention or by combining the features of the present invention with other prior art, falls within the scope of protection of the present invention.

[0022] Unless otherwise specified, all experimental steps or conditions in the examples were performed according to conventional experimental procedures and conditions in the art. Reagents or instruments whose manufacturers are not specified are all commercially available products.

[0023] The reagents used in the embodiments and comparative examples of this invention are as follows: Pyriproxyfen technical grade: purchased from Rudong Zhongyi Chemical Co., Ltd., white powder solid, pyriproxyfen content 98%; Dichlorvos technical grade: purchased from Luohe Xinwang Chemical Co., Ltd., a pale yellow transparent liquid with a dichlorvos content of 95%; Agricultural Milk 600#: The chemical composition is styrene-based phenol polyoxyethylene ether, purchased from Jiangsu Kaiyuan Technology Co., Ltd., and the model is nonionic surfactant 602. EL-40: The chemical composition is polyoxyethylene castor oil, purchased from Nantong Deyi Chemical Co., Ltd., product number: DYTBM / 25; Ammonium dodecylbenzenesulfonate: Purchased from Nantong Deyi Chemical Co., Ltd., product number: DYAY / 01.

[0024] Example 1 This embodiment provides a soluble concentrate containing pyriproxyfen, comprising: 5.1g of pyriproxyfen technical, 78.9g of dichlorvos technical, emulsifiers: 5.6g of agricultural emulsion 600# and 8.4g of EL-40, and stabilizer: 2g of butylated hydroxytoluene.

[0025] This embodiment also provides a method for preparing a soluble concentrate containing pyriproxyfen, comprising the following steps: dissolving 5.1g of pyriproxyfen technical material in 78.9g of dichlorvos technical material, stirring at 400rpm for 20min to completely dissolve the pyriproxyfen in the dichlorvos, then adding the above-mentioned emulsifier and stabilizer and stirring emulsifying at 400rpm for 20min, thereby obtaining a soluble concentrate with a pyriproxyfen content of 5% and a dichlorvos content of 75%.

[0026] Example 2 This embodiment provides a soluble concentrate containing pyriproxyfen, comprising: 1g of pyriproxyfen technical, 80g of dichlorvos technical, emulsifiers: 10g of agricultural emulsion 600# and 8g of ammonium dodecylbenzenesulfonate, and stabilizer: 1g of butylated hydroxytoluene.

[0027] This embodiment also provides a method for preparing a soluble concentrate containing pyriproxyfen, comprising the following steps: dissolving 1g of pyriproxyfen technical material in 80g of dichlorvos technical material, stirring at 300rpm for 30min to completely dissolve the pyriproxyfen in the dichlorvos, then adding the above-mentioned emulsifier and stabilizer and stirring emulsifying at 500rpm for 10min, thereby obtaining a soluble concentrate with a pyriproxyfen content of 1% and a dichlorvos content of 76%.

[0028] Example 3 This embodiment provides a soluble concentrate containing pyriproxyfen, comprising: 10g of pyriproxyfen technical, 70g of dichlorvos technical, emulsifiers: 9.7g of EL-40 and 5.3g of ammonium dodecylbenzenesulfonate, and stabilizer: 5g of butylated hydroxytoluene.

[0029] This embodiment also provides a method for preparing a soluble concentrate containing pyriproxyfen, comprising the following steps: dissolving 10g of pyriproxyfen technical in 70g of dichlorvos technical, stirring at 500rpm for 10min to completely dissolve the pyriproxyfen in the dichlorvos, then adding the above-mentioned emulsifier and stabilizer and stirring emulsifying at 300rpm for 30min, thereby obtaining a soluble concentrate with a pyriproxyfen content of 9.8% and a dichlorvos content of 66.5%.

[0030] Comparative Example 1 This comparative example provides a soluble agent containing pyriproxyfen and its preparation method, which is basically the same as that in Example 1, except that the stabilizer is omitted and the emulsifier is 6.4g of agricultural emulsion 600# and 9.6g of EL-40.

[0031] Comparative Example 2 This comparative example provides a soluble agent containing pyriproxyfen and its preparation method, which is basically the same as that in Example 1, except that the stabilizer is omitted.

[0032] Comparative Example 3 This comparative example provides a soluble agent containing pyriproxyfen and its preparation method, which is basically the same as that in Example 1, except that the emulsifier is omitted.

[0033] Comparative Example 4 This comparative example provides a soluble agent containing pyriproxyfen and its preparation method, which is basically the same as that in Example 3, except that the stabilizer is omitted.

[0034] Experimental Example 1 This experimental example tested the performance indicators of the soluble solvents prepared in each embodiment and comparative example.

[0035] 1. Testing Method (1)Acidity: The acidity of the soluble concentrates prepared in each example and comparative example was determined by referring to GB / T 28135-2011 "Determination Method for Pesticide Acid (Alkali) Content - Indicator Method".

[0036] (2)Initial content: After the soluble concentrates were prepared in each example and comparative example, the contents of pyriproxyfen and dichlorvos were directly determined; The determination of the pyriproxyfen content was carried out by referring to the determination of the pyriproxyfen mass fraction in HG / T 5239-2017 "Industry Standard for Pyriproxyfen Technical". The determination of the dichlorvos content was carried out by referring to the determination of the dichlorvos mass fraction in GB 2549-2003 "Dichlorvos Technical".

[0037] (3)Thermal storage stability: The thermal storage stability of each soluble concentrate was tested by referring to GB / T 19136-2021 "Determination Method for Pesticide Thermal Storage Stability". The soluble concentrates prepared in each example and comparative example were stored at 54 ± 2 °C for 14 days. The contents of pyriproxyfen and dichlorvos in each soluble concentrate after thermal storage were determined by the same method as above to obtain the contents after thermal storage. The decomposition rate was calculated by comparing the contents after thermal storage with the above initial content. The formula is: Decomposition rate = (Initial content - Content after thermal storage) / Initial content × 100%.

[0038] (4)Dilution stability: It was carried out according to Test Method 1 in GB / T 1603-2025 "Determination Method for Pesticide Emulsion Stability". In a 250 mL beaker, 99.5 mL of standard hard water was added. 0.5 mL of the sample was pipetted and slowly added to the standard hard water while stirring continuously to make a 100 mL liquid. After adding the sample, it was stirred at a speed of 3 r / s for 30 s, and immediately transferred to a clean and dry 100 mL graduated cylinder and allowed to stand for 1 h. Observe whether the liquid is homogeneous. If the liquid in the graduated cylinder is homogeneous and there is no precipitate, it is qualified, and the observation result was recorded.

[0039] 2. Test results Table 1 Test results

[0040] As shown in Table 1, the acidities of the examples provided by the present invention were all ≤ 0.3, and in the thermal storage experiment, they all showed better thermal storage stability than all comparative examples, reducing the decomposition rates of the active ingredients of pyriproxyfen and dichlorvos, and also having good stability after dilution, indicating that the soluble concentrate provided by the present invention is a more stable and efficient compounding scheme of pyriproxyfen and dichlorvos.

[0041] Obviously, the above embodiments are merely illustrative examples for clear explanation and are not intended to limit the implementation. Those skilled in the art will recognize that other variations or modifications can be made based on the above description. It is neither necessary nor possible to exhaustively list all possible implementations here. However, obvious variations or modifications derived therefrom are still within the scope of protection of this invention.

Claims

1. A soluble solvent containing pyriproxyfen, characterized in that, By weight, it includes: 1-10 parts of pyriproxyfen technical, 70-80 parts of dichlorvos technical, 10-20 parts of emulsifier, and 1-5 parts of stabilizer.

2. The pyriproxyfen-containing soluble agent according to claim 1, characterized in that, The emulsifier includes at least one of ammonium dodecylbenzenesulfonate, polyoxyethylene castor oil, and styrene-phenol polyoxyethylene ether; And / or, the stabilizer includes at least one of butylated hydroxytoluene, tert-butylhydroquinone, and butylated hydroxyanisole.

3. The pyriproxylic acid-containing soluble agent according to claim 1 or 2, characterized in that, The product comprises, by weight: 10 parts of pyriproxyfen technical, 70 parts of dichlorvos technical, 15 parts of emulsifier, and 5 parts of stabilizer, wherein the emulsifier is polyoxyethylene castor oil and ammonium dodecylbenzenesulfonate in a mass ratio of 1-2:1, and the stabilizer is butylated hydroxytoluene.

4. The pyriproxyfen-containing soluble agent according to claim 1 or 2, characterized in that, The product comprises, by weight: 5.1 parts of pyriproxyfen technical, 78.9 parts of dichlorvos technical, 14 parts of emulsifier, and 2 parts of stabilizer, wherein the emulsifier is styrene-phenol polyoxyethylene ether and polyoxyethylene castor oil in a mass ratio of 1:1-2, and the stabilizer is butylated hydroxytoluene.

5. The pyriproxyfen-containing soluble agent according to claim 1 or 2, characterized in that, The product comprises, by weight: 1 part pyriproxyfen technical, 80 parts dichlorvos technical, 18 parts emulsifier, and 1 part stabilizer, wherein the emulsifier is styrene-phenol polyoxyethylene ether and ammonium dodecylbenzenesulfonate in a mass ratio of 1-2:1, and the stabilizer is butylated hydroxytoluene.

6. The pyriproxypropyl soluble agent according to claim 1, characterized in that, The pyriproxyfen technical grade contains ≥98% pyriproxyfen.

7. The pyriproxylic acid-containing soluble agent according to claim 1, characterized in that, The dichlorvos technical grade contains ≥95% dichlorvos.

8. The method for preparing the pyriproxypropyl soluble solvent according to any one of claims 1-7, characterized in that, The process includes the following steps: mixing pyriproxyfen technical and dichlorvos technical, adding emulsifier and stabilizer for emulsification, to obtain a soluble concentrate containing pyriproxyfen.

9. The method for preparing the pyriproxylic acid-containing soluble agent according to claim 8, characterized in that, The mixing speed is 300-500 rpm, and the time is 10-30 min.

10. The method for preparing the pyriproxylic acid-containing soluble agent according to claim 8, characterized in that, The emulsification speed is 300-500 rpm, and the time is 10-30 min.

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