A pesticide synergist and a method for preparing the same

Abstract

The application discloses a pesticide synergist and a preparation method thereof. The pesticide synergist comprises a silanol-initiated polyether shown in formula I, an inositol phosphate-initiated polyether shown in formula II, an alcohol auxiliary agent and water. The silanol-initiated polyether shown in formula I and the inositol phosphate-initiated polyether shown in formula II are synergized, so that the adhesion, spreading, penetration and retention capacity of pesticide droplets on a target surface are significantly enhanced, and the utilization rate of the pesticide is effectively improved. The product has the advantages of low toxicity, environmental friendliness, multi-functional synergism, wide compatibility and the like, the preparation process is simple and stable, and the product is suitable for industrial production.

Description

Technical Field

[0001] This invention relates to the field of pesticide adjuvant technology, and more specifically, to a pesticide synergist and its preparation method, particularly a pesticide synergist with low toxicity, environmental friendliness, high efficiency and multifunctionality, used to improve the adhesion, spreading, penetration and retention of pesticides on the target surface, thereby improving pesticide utilization and reducing environmental pollution. Background Technology

[0002] Pesticides play an irreplaceable role in modern agricultural production; however, traditional pesticides suffer from problems such as low utilization rate, serious environmental pollution, and poor target deposition. Statistics show that the effective utilization rate of pesticides using traditional application methods is generally below 30%, with large amounts of pesticide solution lost during spraying due to evaporation, drift, and rolling, resulting not only in resource waste but also potential risks to the ecological environment and non-target organisms.

[0003] To improve pesticide utilization efficiency, pesticide synergists are widely used as an important auxiliary method. In existing technologies, pesticide synergists mostly use organosilicon, vegetable oil, and surfactants as their main components, improving efficacy by reducing the surface tension of the pesticide solution and enhancing its wetting and spreading ability. However, these synergists still have certain limitations in practical applications: for example, some organosilicon adjuvants can easily cause phytotoxicity to certain crops and have poor biodegradability; while vegetable oil adjuvants are environmentally friendly, their synergistic effects are limited, especially in terms of rain resistance and penetration; furthermore, traditional synergists have limited functionality and cannot simultaneously meet multiple requirements such as anti-evaporation, anti-drift, rapid penetration, and long-lasting retention.

[0004] In recent years, although some studies have attempted to improve the performance of synergists by compounding multiple surfactants or introducing natural ingredients, such as the insecticide synergist containing plant essential oils disclosed in CN120660688A and the ammonium sulfate-siloxane composite synergist system for herbicides involved in CN120642853A, their synergistic effect, environmental safety and multifunctional integration still need to be improved.

[0005] Therefore, developing a novel synergist that combines low toxicity, high degradability, multifunctional synergistic effects, and applicability to various pesticide formulations has become an urgent technical problem to be solved in the field of pesticide adjuvants. Summary of the Invention

[0006] In view of the needs and shortcomings of the existing technology, the present invention provides a pesticide synergist and its preparation method by synergistic compounding of polyethers initiated by silanol and polyether surfactants initiated by inositol phosphate. The pesticide synergist can significantly improve the adhesion, spreading, penetration and retention of pesticide droplets on the target surface, thereby improving pesticide utilization and reducing environmental pollution. It has the characteristics of low toxicity, environmental friendliness, high efficiency and multifunctionality.

[0007] This invention is achieved through the following technical solution:

[0008] In a first aspect, the present invention provides a pesticide synergist, comprising, by weight parts: 1 to 60 parts of a silanol-based polyether as shown in Formula I, 1 to 50 parts of an inositol phosphate-based polyether as shown in Formula II, 1 to 30 parts of an alcohol adjuvant, and 1 to 80 parts of water.

[0009] The silanol-based polyether has the structure shown in Formula I:

[0010]

[0011] Formula I

[0012] In Equation 1:

[0013] R1, R2, and R3 are each independently selected from C1-C 12 Alkyl or C6-C 12 Aryl; each R4 is independently selected from H, methyl, or ethyl;

[0014] n is an integer from 1 to 350;

[0015] The inositol phosphate-based polyether has the structure shown in Formula II:

[0016]

[0017] Formula II

[0018] In Formula II:

[0019] Each R5 is independently selected from H, -P(=O)(OR6)(OR7) or -(CH2CH(R8)O). m -H;

[0020] Each of R6 and R7 is independently selected from H, C1-C4 alkyl groups, or -(CH2CH(R8)O). m -H;

[0021] Furthermore, formula II contains at least one -(CH2CH(R8)O) m -H;

[0022] Each R8 is independently selected from H, methyl, or ethyl;

[0023] Each m is an independent integer from 1 to 150.

[0024] In some embodiments, in Formula I: R1, R2, and R3 are each independently selected from C1-C8 alkyl, phenyl, preferably methyl, ethyl, propyl, or phenyl; more preferably ethyl.

[0025] In some implementations, in Equation I, n takes the value of an integer from 10 to 150.

[0026] In some embodiments, in Formula I: the polyether chain is a random copolymer, block copolymer, or gradient copolymer; preferably a block copolymer structure.

[0027] In some embodiments, in Formula I: R1, R2, and R3 are all ethyl groups, and m is an integer from 10 to 150 (e.g., an integer from 40 to 65).

[0028] In some embodiments, in Formula I: R1, R2, and R3 are all methyl groups, and m is an integer from 10 to 150 (e.g., an integer from 40 to 65).

[0029] In some embodiments, in Formula I: R1 and R2 are methyl, R3 is phenyl, and m is an integer from 10 to 150 (e.g., an integer from 40 to 65).

[0030] In some embodiments, in Formula I: R1, R2, and R3 are all phenyl groups, and n is an integer from 10 to 150 (e.g., an integer from 40 to 65).

[0031] In some embodiments, in Formula II: there are two, three, four, five or six R5s that are simultaneously -P(=O)(OR6)(OR7), wherein each R6 and R7 is independently selected from hydrogen, C1-C4 alkyl or -(CH2CH(R8)O). m -H; the remaining R5 groups are H or -(CH2CH(R8)O) m -H; each R8 is independently selected from H, methyl, ethyl; m is an integer from 10 to 150, and can be an integer from 10 to 60 (e.g., 30).

[0032] In some embodiments, the pesticide synergist comprises, by weight parts: 8 to 50 parts of silanol-based polyether, 8 to 40 parts of inositol phosphate-based polyether, 5 to 15 parts of alcohol adjuvant, and 30 to 80 parts of water.

[0033] In some embodiments, the pesticide synergist comprises, by weight parts: 10 to 40 parts of silanol-based polyether, 10 to 30 parts of inositol phosphate-based polyether, 5 to 10 parts of alcohol adjuvant, and 40 to 60 parts of water.

[0034] In some embodiments, the pesticide synergist comprises, by weight parts: 20 parts of silanol-based polyether, 15 parts of inositol phosphate-based polyether, 5 parts of alcohol adjuvant, and 60 parts of water.

[0035] In some embodiments, the pesticide synergist comprises, by weight parts: 30 parts of silanol-based polyether, 20 parts of inositol phosphate-based polyether, 8 parts of alcohol adjuvant, and 42 parts of water.

[0036] In some embodiments, the pesticide synergist comprises, by weight parts: 40 parts of silanol-based polyether, 10 parts of inositol phosphate-based polyether, 10 parts of alcohol adjuvant, and 40 parts of water.

[0037] In some embodiments, the pesticide synergist comprises, by weight parts: 10 parts of silanol-based polyether, 30 parts of inositol phosphate-based polyether, 6 parts of alcohol adjuvant, and 54 parts of water.

[0038] The silanol-based polyether can be prepared by the following method:

[0039] Using silanol as an initiator, etherification is achieved by an addition reaction with epoxides in the presence of a basic catalyst.

[0040] In some embodiments, the alkaline catalyst is selected from sodium hydroxide, lithium hydroxide, or potassium hydroxide, preferably potassium hydroxide; the amount of the alkaline catalyst is 0.1% to 1% of the total mass of the reaction raw materials, preferably 0.3% to 0.5%.

[0041] In some embodiments, the silanol is selected from one or more combinations of trimethylsilanol, triethylsilanol, tripropylsilanol, tributylsilanol, triphenylsilanol, etc., preferably one or a combination of trimethylsilanol and triethylsilanol, and more preferably triethylsilanol.

[0042] In some embodiments, the epoxide is selected from one or more combinations of ethylene oxide, propylene oxide, and butane oxide.

[0043] In some embodiments, the molar ratio of the silanol, propylene oxide, ethylene oxide, and butyl oxide is 1:(0 to 100):(1 to 200):(0 to 50).

[0044] In some embodiments, the epoxide is one or a combination of ethylene oxide and propylene oxide.

[0045] In some embodiments, the molar ratio of the silanol, propylene oxide and ethylene oxide is 1:(0 to 100):(1 to 200).

[0046] In some embodiments, the temperature of the addition reaction is 80°C to 150°C, preferably 120°C to 130°C.

[0047] In some embodiments, the reaction time of the addition reaction is 2 to 8 hours, preferably 4 to 6 hours.

[0048] The inositol phosphate-based polyether can be prepared by the following method:

[0049] Using one or more of inositol phosphate esters as initiators, etherification is achieved by addition reaction with epoxides in the presence of a basic catalyst.

[0050] In some embodiments, the alkaline catalyst is selected from sodium hydroxide, lithium hydroxide, or potassium hydroxide, preferably potassium hydroxide; the amount of the alkaline catalyst is 0.1% to 1% of the total mass of the reaction raw materials, preferably 0.3% to 0.5%.

[0051] In some embodiments, the inositol phosphate is selected from inositol hexaphosphate, or an inositol phosphate composition containing 2 to 6 phosphate groups derived from inositol hexaphosphate by partial esterification or hydrolysis, the composition encompassing all possible positional isomers thereof and mixtures thereof, wherein the phosphate groups are -P(=O)(OR) a (OR) b ), each R a R b Each is independently selected from H or C1-C4 alkyl groups.

[0052] In some embodiments, the inositol phosphate is selected from at least one or more combinations of inositol diphosphate, inositol diphosphate, inositol triphosphate, inositol tetraphosphate, inositol pentaphosphate, and inositol hexaphosphate.

[0053] In some embodiments, the epoxide is selected from at least one or more combinations of ethylene oxide, propylene oxide, butane oxide, etc.

[0054] In some embodiments, the molar ratio of inositol phosphate, propylene oxide, ethylene oxide and butyl oxide is 1:(0 to 50):(1 to 100):(0 to 50).

[0055] In some embodiments, the epoxide is one or a combination of ethylene oxide and propylene oxide.

[0056] In some embodiments, the molar ratio of inositol phosphate, propylene oxide and ethylene oxide is 1:(0 to 50):(1 to 100), and optionally 1:(10 to 40):(10 to 50).

[0057] In some embodiments, the temperature of the addition reaction is 80°C to 150°C, preferably 120°C to 130°C.

[0058] In some embodiments, the addition reaction takes 2 to 8 hours, preferably 4 to 6 hours.

[0059] In some embodiments, the alcohol auxiliary is selected from at least one of methanol, ethanol, propanol, butanol, ethylene glycol, propylene glycol, glycerol, etc., preferably propylene glycol or glycerol.

[0060] Secondly, the present invention provides a method for preparing a pesticide synergist, comprising:

[0061] The polyether is prepared by mixing silanol-based polyether, inositol phosphate-based polyether, alcohol additives, and water.

[0062] The definitions and dosages of the silanol-based polyethers, inositol phosphate-based polyethers, and alcohol-based auxiliaries are as described in the first aspect.

[0063] In some embodiments, the method for preparing the pesticide synergist includes:

[0064] The polyether starting with silanol, the polyether starting with inositol phosphate, alcohol additives and water are stirred at 25 ℃ to 40 ℃ for 40 min to 60 min until well mixed.

[0065] Compared with the prior art, the technical solution of this application has the following beneficial effects:

[0066] 1. Low toxicity and environmental safety: The selected raw materials, silanol and inositol phosphate, have good environmental compatibility, are easy to degrade, are safe for non-target organisms, and meet the requirements of green agriculture development.

[0067] 2. High Efficiency and Multifunctionality: The synergist of this invention achieves complementary and enhanced performance through the synergistic compounding of silanol-based polyethers and inositol phosphate-based polyethers. The silanol-based polyether molecules contain hydrophobic organosilicon segments, which can form a highly effective adsorption film on droplet surfaces and at gas-liquid interfaces, significantly reducing surface tension and endowing the drug solution with excellent anti-evaporation and anti-drift capabilities. The inositol phosphate-based polyether molecules are rich in phosphate groups and hydrophilic polyether chains. Its phosphate structure exhibits strong affinity and adsorption for biological surfaces such as plant leaves, while the polyether segments provide excellent wetting and penetration. Together, they ensure rapid wetting and spreading of the drug solution, rapid penetration, and firm adhesion to the target surface, thus demonstrating excellent resistance to rain erosion. The synergistic effect of these two components gives it multiple functions, achieving "one agent, multiple effects."

[0068] 3. Significant synergistic effect: This synergist can effectively reduce the surface tension of pesticide droplets, promote the adhesion and penetration of pesticide solution on plant leaves and insect bodies, greatly improve the effective utilization rate of pesticides, and thus allow for a reduction in the amount of original pesticide used.

[0069] 4. Wide compatibility: It has good compatibility with most commonly used pesticides (such as insecticides, fungicides, and herbicides) and adjuvants, and is not prone to antagonistic effects, making it widely applicable.

[0070] 5. Mature and stable process: The preparation method is simple, the reaction conditions are mild, it is easy to realize industrial production, and the quality control is stable. Attached Figure Description

[0071] Figure 1 This is the 1H NMR spectrum of the silanol-based polyether prepared in the embodiments of this application.

[0072] Figure 2 This is the 1H NMR spectrum of the inositol phosphate-based polyether prepared in the embodiments of this application.

[0073] Figure 3 This is the surface tension test result of the pesticide synergist in Test Example 2.

[0074] Figure 4 The results are from the leaf spreading test after the addition of an synergist to the herbal solution in Example 2. Detailed Implementation

[0075] To make the original intent, technical solutions, and technical effects of the embodiments of the present invention clearer, the technical solutions are described clearly and completely below in conjunction with the embodiments; obviously, the described embodiments are some embodiments of the present invention, but 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.

[0076] Unless otherwise specified, all reagents and instruments used in the following examples and comparative examples are commercially available.

[0077] Reagents and sources:

[0078] Triethylsilanol: Purity ≥98%, Shanghai Maclean Biochemical Technology Co., Ltd.;

[0079] Trimethylsilanol: Purity ≥98%, Aladdin Reagent (Shanghai) Co., Ltd.;

[0080] Tributylsilanol: Purity ≥97%, Tianjin Kemeo Chemical Reagent Co., Ltd.;

[0081] Triphenylsilanol: Purity ≥98%, Sigma-Aldrich Reagents Company;

[0082] Ethylene oxide: purity ≥ 99.5%, Suzhou Huasu Chemical Co., Ltd.;

[0083] Propylene oxide: purity ≥ 99.5%, Shandong Binhua Group Co., Ltd.;

[0084] Butane oxide: purity ≥98%, Shanghai Puzhen Biotechnology Co., Ltd.;

[0085] Potassium hydroxide: analytical grade, Sinopharm Chemical Reagent Co., Ltd.;

[0086] Inositol diphosphate ester: purity ≥95%, Wuhan Yuancheng Gongchuang Technology Co., Ltd.;

[0087] Inositol triphosphate: purity ≥95%, Shanghai Yuanye Biotechnology Co., Ltd.;

[0088] Inositol pentaphosphate: Purity ≥90%, Chengdu Pufeed Biotechnology Co., Ltd.;

[0089] Inositol hexaphosphate: purity ≥98%, Zhengzhou Alpha Chemical Co., Ltd.;

[0090] Ethanol: Analytical grade, Sinopharm Chemical Reagent Co., Ltd.;

[0091] Propylene glycol: analytical grade, Shanghai Lingfeng Chemical Reagent Co., Ltd.;

[0092] Glycerol: Analytical grade, Tianjin Yongda Chemical Reagent Co., Ltd.;

[0093] Butanol: Analytical grade, Guangdong Guanghua Technology Co., Ltd.;

[0094] Methanol: Analytical grade, Sinopharm Chemical Reagent Co., Ltd.

[0095] 1H NMR: Measured using a Bruker Avance 400 MHz instrument. The sample was dissolved in deuterated chloroform.

[0096] Example 1: Preparation of pesticide synergist 1

[0097] (1) Synthesis of polyethers starting from silanol: Triethylsilanol was used as the initiator, and the molar ratio of triethylsilanol, propylene oxide (PO), and ethylene oxide (EO) was 1:22:29. Potassium hydroxide was used as the catalyst, and the amount of catalyst added was 0.3% of the total mass of the raw materials. The mixture was stirred at 300~500 rpm at 120 °C to ensure uniform contact of the reactants, controllable heat transfer, and safe and complete reaction. After 4 hours of reaction, an appropriate amount of phosphoric acid was added to neutralize the reaction solution to a pH of 6~7 and then purified: the mixture was distilled at 100~120 °C for 1~2 hours to remove unreacted alkylene oxide monomers, water, and light components. An appropriate amount of anhydrous sodium sulfate was added for dehydration, and the mixture was filtered. After adsorption purification through an adsorption column packed with activated carbon, it was filtered again (optional) and cooled to room temperature to obtain polyethers starting from silanol.

[0098] (2) Synthesis of polyethers starting from inositol phosphate: Inositol triphosphate was used as the initiator, with a molar ratio of inositol triphosphate, propylene oxide, and ethylene oxide of 1:22:29. Potassium hydroxide was used as the catalyst, and the amount of catalyst added was 0.3% of the total mass of the raw materials. The mixture was stirred at 300-500 rpm at 120 °C to ensure uniform contact of the reactants, controllable heat transfer, and safe and complete reaction. After 4 hours of reaction, an appropriate amount of phosphoric acid was added to neutralize the reaction solution to a pH of 6-7 and then purified. The mixture was distilled at 100-120 °C for 1-2 hours to remove residual monomers and light components. Anhydrous sodium sulfate was added for dehydration, and the mixture was filtered. After adsorption purification through an adsorption column packed with activated carbon, it was filtered again (optional) and cooled to room temperature to obtain polyethers starting from inositol phosphate.

[0099] (3) Preparation of synergist: by weight ratio, 20 parts of polyether starting with silanol, 15 parts of polyether starting with inositol phosphate, 5 parts of ethanol and 60 parts of water; stir the above raw materials at 30 ℃ at 200~400 rpm for 40 minutes, mix evenly, and obtain pesticide synergist 1.

[0100] Example 2: Preparation of pesticide synergist 2

[0101] (1) Synthesis of polyethers starting from silanol: A mixed silanol of trimethylsilanol and triethylsilanol (mass ratio 1:1) was used as the starting agent. The molar ratio of the mixed silanol, propylene oxide and ethylene oxide was 1:0.924:2.436. Potassium hydroxide was used as the catalyst, and the amount of catalyst added was 0.4% of the total mass of the raw materials. The mixture was stirred at 300~500 rpm at 125 °C to ensure uniform contact of the reactants, controllable heat transfer, and safe and complete reaction. After 5 hours of reaction, an appropriate amount of phosphoric acid was added to neutralize the reaction solution to a pH of 6~7 and then purified. The mixture was distilled at 100~120 °C for 1~2 hours to remove residual monomers and light components. Anhydrous sulfuric acid was added for dehydration, and the mixture was filtered, purified by adsorption through an adsorption column packed with activated carbon, filtered again (optional), and cooled to room temperature to obtain polyethers starting from inositol phosphate.

[0102] (2) Synthesis of polyethers starting from inositol phosphate: A mixture of inositol diphosphate and inositol triphosphate (mass ratio 1:1) was used as the starting agent. The molar ratio of the mixed inositol phosphate, propylene oxide, and ethylene oxide was 1:3.24:8.53. Potassium hydroxide was used as the catalyst, and the amount of catalyst added was 0.4% of the total mass of the raw materials. The mixture was stirred at 300~500 rpm at 125 °C to ensure uniform contact of the reactants, controllable heat transfer, and safe and complete reaction. After 5 hours of reaction, an appropriate amount of phosphoric acid was added to neutralize the reaction solution to a pH of 6~7 and then purified. The mixture was distilled at 100~120 °C for 1~2 hours to remove residual monomers and light components. Anhydrous sulfuric acid was added for dehydration, followed by filtration, adsorption purification through an adsorption column packed with activated carbon, and then filtration again (optional). The mixture was cooled to room temperature to obtain polyethers starting from inositol phosphate.

[0103] (3) Preparation of synergist: by weight ratio, 30 parts of polyether starting with silanol, 20 parts of polyether starting with inositol phosphate, 8 parts of propylene glycol, and 42 parts of water; stir the above raw materials at 35 ℃ at 200~400 rpm for 50 minutes, mix evenly, and obtain pesticide synergist 2.

[0104] Example 3: Preparation of pesticide synergist 3

[0105] (1) Synthesis of polyethers starting from silanol: Tributylsilanol was used as the initiator, with a molar ratio of 1:0:150 for tributylsilanol, propylene oxide, and ethylene oxide. Sodium hydroxide was used as the catalyst, and the amount of catalyst added was 0.5% of the total mass of the raw materials. The mixture was stirred at 300-500 rpm at 130°C to ensure uniform contact of the reactants, controllable heat transfer, and safe and complete reaction. After 6 hours of reaction, an appropriate amount of phosphoric acid was added to neutralize the reaction solution to a pH of 6-7 and then purified. The mixture was distilled at 100-120°C for 1-2 hours to remove residual monomers and light components. Anhydrous sulfuric acid was added for dehydration, followed by filtration, adsorption purification through an adsorption column packed with activated carbon, and then filtration again (optional). The mixture was cooled to room temperature to obtain polyethers starting from inositol phosphate.

[0106] (2) Synthesis of polyethers starting from inositol phosphate: Inositol hexaphosphate was used as the initiator, with a molar ratio of inositol hexaphosphate, propylene oxide, and ethylene oxide of 1:0:150. Sodium hydroxide was used as the catalyst, and the amount of catalyst added was 0.5% of the total mass of the raw materials. The mixture was stirred at 300-500 rpm at 130 °C to ensure uniform contact of the reactants, controllable heat transfer, and safe and complete reaction. After 6 hours of reaction, an appropriate amount of phosphoric acid was added to neutralize the reaction solution to a pH of 6-7 and then purified. The mixture was distilled at 100-120 °C for 1-2 hours to remove residual monomers and light components. Anhydrous sulfuric acid was added for dehydration, followed by filtration, adsorption purification through an adsorption column packed with activated carbon, and then filtration again (optional). The mixture was cooled to room temperature to obtain polyethers starting from inositol phosphate.

[0107] (3) Preparation of synergist: by weight ratio, 40 parts of polyether starting with silanol, 10 parts of polyether starting with inositol phosphate, 10 parts of glycerol, and 40 parts of water; stir the above raw materials at 200~400 rpm for 60 minutes at 40 ℃ until they are evenly mixed to obtain pesticide synergist 3.

[0108] Example 4: Preparation of pesticide synergist 4

[0109] (1) Synthesis of polyethers starting from silanol: Triphenylsilanol was used as the initiator, with a molar ratio of triphenylsilanol, propylene oxide, and ethylene oxide of 1:36:29. Lithium hydroxide was used as the catalyst, and the catalyst dosage was 0.2% of the total mass of the raw materials. The mixture was stirred at 300-500 rpm at 110°C to ensure uniform contact of the reactants, controllable heat transfer, and safe and complete reaction. After 3 hours of reaction, an appropriate amount of phosphoric acid was added to neutralize the reaction solution to a pH of 6-7 and then purified. The mixture was distilled at 100-120°C for 1-2 hours to remove residual monomers and light components. Anhydrous sulfuric acid was added for dehydration, followed by filtration, adsorption purification through an adsorption column packed with activated carbon, and then filtration again (optional). The mixture was cooled to room temperature to obtain polyethers starting from inositol phosphate.

[0110] (2) Synthesis of polyethers starting from inositol phosphate: Inositol triphosphate was used as the initiator, with a molar ratio of inositol triphosphate, propylene oxide, and ethylene oxide of 1:20:25. Lithium hydroxide was used as the catalyst, and the catalyst dosage was 0.2% of the total mass of the raw materials. The mixture was stirred at 300-500 rpm at 110 °C to ensure uniform contact of the reactants, controllable heat transfer, and safe and complete reaction. After 3 hours of reaction, an appropriate amount of phosphoric acid was added to neutralize the reaction solution to a pH of 6-7 and then purified. The mixture was distilled at 100-120 °C for 1-2 hours to remove residual monomers and light components. Anhydrous sulfuric acid was added for dehydration, followed by filtration, adsorption purification through an adsorption column packed with activated carbon, and then filtration again (optional). The mixture was cooled to room temperature to obtain polyethers starting from inositol phosphate.

[0111] (3) Preparation of synergist: by weight ratio, 10 parts of polyether starting with silanol, 30 parts of polyether starting with inositol phosphate, 6 parts of butanol, and 54 parts of water; stir the above raw materials at 200~400 rpm for 30 minutes at 25 ℃ until they are evenly mixed to obtain pesticide synergist 4.

[0112] Example 5: Preparation of Synergist 5

[0113] (1) Synthesis of polyethers starting from silanol: A mixture of trimethylsilanol, tripropylsilanol and tributylsilanol (mass ratio 1:1:1) was used as the starting agent. Ethylene oxide, propylene oxide and butane oxide were copolymerized. The molar ratio of the mixed silanol, ethylene oxide, propylene oxide and butane oxide was 1:100:200:50. Potassium hydroxide was used as the catalyst and the amount of catalyst added was 1.0% of the total mass of the raw materials. The stirring was carried out at 150 °C and the stirring speed was 300~500 rpm to ensure uniform contact of reactants, controllable heat transfer and safe and complete reaction. After reacting for 8 hours, add an appropriate amount of phosphoric acid to neutralize the reaction solution to a pH of 6-7 and purify it. Distill at 100-120 °C for 1-2 hours to remove residual monomers and light components. Add anhydrous sulfuric acid to dehydrate, filter, and purify by adsorption through an adsorption column packed with activated carbon. Filter again (optional) and cool to room temperature to obtain polyether starting with inositol phosphate.

[0114] (2) Synthesis of polyethers starting from inositol phosphate: A mixture of inositol diphosphate, inositol tetraphosphate and inositol pentaphosphate (mass ratio 1:1:1) was used as the starting agent. Ethylene oxide, propylene oxide and butylene oxide were copolymerized. The molar ratio of the mixed inositol phosphate, ethylene oxide, propylene oxide and butylene oxide was 10:15:39:12. Potassium hydroxide was used as the catalyst and the amount of catalyst added was 1.0% of the total mass of the raw materials. The stirring was carried out at 150 °C at a stirring speed of 300~500 rpm to ensure uniform contact of reactants, controllable heat transfer and safe and complete reaction. After reacting for 8 hours, add an appropriate amount of phosphoric acid to neutralize the reaction solution to a pH of 6-7 and purify it. Distill at 100-120 °C for 1-2 hours to remove residual monomers and light components. Add anhydrous sulfuric acid to dehydrate, filter, and purify by adsorption through an adsorption column packed with activated carbon. Filter again (optional) and cool to room temperature to obtain polyether starting with inositol phosphate.

[0115] (3) Preparation of synergist: by weight ratio, 60 parts of polyether starting with silanol, 50 parts of polyether starting with inositol phosphate, 1 part of methanol, and 1 part of water; stir the above raw materials at 35 ℃ at 200~400 rpm for 45 minutes, mix evenly, and obtain pesticide synergist 5.

[0116] Comparative Example 1: Preparation of Pesticide Synergist 6

[0117] (1) Synthesis of polyethers starting with silanol: The synthesis of polyethers starting with silanol was carried out according to step (1) of Example 2.

[0118] (2) Preparation of synergist: by weight ratio, 50 parts of polyether starting with silanol, 8 parts of propylene glycol, and 42 parts of water; stir and mix the above raw materials at 35 ℃ at 200~400 rpm for 50 minutes until they are evenly mixed to obtain pesticide synergist 6.

[0119] Comparative Example 2: Preparation of Pesticide Synergist 7

[0120] (1) Synthesis of polyethers starting from inositol phosphate: The synthesis of polyethers starting from inositol phosphate was carried out according to step (2) of Example 2.

[0121] (2) Preparation of synergist: by weight ratio, 50 parts of polyether starting with inositol phosphate, 8 parts of propylene glycol, and 42 parts of water; stir and mix the above raw materials at 200~400 rpm at 35℃ for 50 minutes until they are evenly mixed to obtain pesticide synergist 7.

[0122] Test Example 1: Compatibility Test of Synergist and Pesticide

[0123] The compatibility of the pesticide synergist of this application with pesticides was tested, using herbicides such as benzocaproic acid and insecticides such as lambda-cyhalothrin.

[0124] Compatibility testing:

[0125] The synergists of the examples and comparative examples were mixed with benzoxazine and lambda-cyhalothrin at a ratio of 1:20 at room temperature, 0°C or 40°C, respectively, and allowed to stand for 24 hours. The shapes were observed and the results are shown in Table 1 below.

[0126] Table 1.

[0127]

[0128] Test Example 2: Synergistic Effect Test of Pesticide Synergists

[0129] The pesticide synergist prepared in Examples 1 to 5 above, a commercially available organosilicon synergist (active ingredient: polyether-modified trisiloxane, content 10%), or a commercially available vegetable oil synergist (active ingredient: soybean oil methyl ester, content 80%) is compounded with the pesticide benzoyl permethrin. The specific preparation method is as follows:

[0130] Test solution group: Dissolve benzoyl sulfadiazine in water to prepare a solution with a concentration of 0.1%; add 5% of the pesticide synergist prepared in Examples 1 to 5 according to the mass percentage, and mix well.

[0131] Blank group: The tested pesticide was directly prepared at a concentration of 0.1% without the addition of any synergists.

[0132] (1) Measurement of surface tension of drug solution:

[0133] Referring to the ring film-forming method in GB / T 5549—2010, a certain amount of the test drug solution was taken and shaken well at room temperature (20±0.5)℃, and the surface tension was measured on a surface tension meter. The blank group was used as a control.

[0134] (2) Method for determining the contact angle and spreading properties of the drug solution: In a closed environment, 5 μL of the test drug solution was taken and the instantaneous contact angle and spreading diameter of the droplet were measured on a contact angle measuring instrument (JC2000D3 type). The blank group was used as a control.

[0135] (3) Method for determining the permeability of the drug solution: The permeability of the drug solution was determined according to the method of national standard HG / T 2575—1994. After shaking the test drug solution well, it was poured into 50 mL beakers. Clean canvas sheets were placed above the beakers containing each treatment drug solution, so that each canvas sheet fell naturally from the same height. The time required for the canvas sheet to go from contacting the drug solution to being completely immersed in the drug solution was recorded with a stopwatch. Distilled water was used as a control.

[0136] result:

[0137] The surface tension test results of the test solution are shown in the figure. Figure 3The surface tension of the pesticide solutions prepared in Examples 1 to 5 with 0.03% or more of the pesticide synergist added was all below 28 mN / m, indicating that the pesticide synergist of this application can significantly reduce the surface tension of the pesticide solution at a low addition amount.

[0138] The results of the contact angle and spreadability tests of the test solution are shown in the figure. Figure 4 The results showed that the contact angle of the blank group on plant leaves was 72.5°, while the contact angle of the pesticide solution with 5% of the pesticide synergist prepared in Examples 1 to 5 was less than 65° on plant leaves.

[0139] The pesticide utilization rate was 30%-50% higher than that of the control group, with no obvious pesticide damage and excellent environmental safety.

[0140] The above description is merely a specific embodiment of the present invention, but the scope of protection of the present invention is not limited thereto. Any variations or substitutions that can be easily conceived by those skilled in the art within the technical scope disclosed in the present invention should be included within the scope of protection of the present invention. Therefore, the scope of protection of the present invention should be determined by the scope of the claims.

Claims

1. A pesticide synergist, characterized in that, The pesticide synergist, by weight, comprises: 1 to 60 parts of a silanol-based polyether as shown in Formula I, 1 to 50 parts of an inositol phosphate-based polyether as shown in Formula II, 1 to 30 parts of an alcohol adjuvant, and 1 to 80 parts of water. The silanol-based polyether has the structure shown in Formula I: Formula I In Equation 1: R1, R2, and R3 are each independently selected from C1-C 12 Alkyl or C6-C 12 Aryl; each R4 is independently selected from H, methyl, or ethyl; n is an integer from 1 to 350; The inositol phosphate-based polyether has the structure shown in Formula II: Formula II In Formula II: Each R5 is independently selected from H, -P(=O)(OR6)(OR7) or -(CH2CH(R8)O). m -H; Each of R6 and R7 is independently selected from H, C1-C4 alkyl groups, or -(CH2CH(R8)O). m -H; Furthermore, formula II contains at least one -(CH2CH(R8)O) m -H; each R8 is independently selected from H, methyl, or ethyl; Each m is an independent integer from 1 to 150.

2. The pesticide synergist according to claim 1, characterized in that, In Formula I: R1, R2, and R3 are each independently selected from C1-C8 alkyl, phenyl, preferably methyl, ethyl, propyl, or phenyl; more preferably ethyl; and / or n is an integer from 10 to 150; and / or The polyether chain is a random copolymer, block copolymer, or gradient copolymer; preferably a block copolymer structure.

3. The pesticide synergist according to claim 1 or 2, characterized in that, In Formula I: R1, R2, and R3 are all ethyl groups, and n is an integer from 10 to 150 (e.g., an integer from 40 to 65); or R1, R2, and R3 are all methyl groups, and m is an integer from 10 to 150 (e.g., an integer from 40 to 65); or R1 and R2 are methyl, R3 is phenyl, and m is an integer from 10 to 150 (e.g., an integer from 40 to 65); or R1, R2, and R3 are all phenyl groups, and m is an integer from 10 to 150 (e.g., an integer from 40 to 65).

4. The pesticide synergist according to claim 1 or 2, characterized in that, In Formula II: there are two, three, four, five or six R5s that are simultaneously -P(=O)(OR6)(OR7), wherein each R6 and R7 is independently selected from hydrogen, C1-C4 alkyl or -(CH2CH(R8)O). m -H; the remaining R5 groups are H or -(CH2CH(R8)O) m -H; each R8 is independently selected from H, methyl, ethyl; m is an integer from 10 to 150, and can be an integer from 10 to 60 (e.g., 30).

5. The pesticide synergist according to any one of claims 1-4, characterized in that, The pesticide synergist, by weight, comprises: 8 to 50 parts of silanol-based polyether, 8 to 40 parts of inositol phosphate-based polyether, 5 to 15 parts of alcohol adjuvant, and 30 to 80 parts of water.

6. The pesticide synergist according to claim 5, characterized in that, The pesticide synergist, by weight parts, comprises: 10 to 40 parts of silanol-based polyether, 10 to 30 parts of inositol phosphate-based polyether, 5 to 10 parts of alcohol adjuvant, and 40 to 60 parts of water; or The pesticide synergist, by weight, comprises: 20 parts of silanol-based polyether, 15 parts of inositol phosphate-based polyether, 5 parts of alcohol adjuvant, and 60 parts of water; or The pesticide synergist, by weight, comprises: 30 parts of silanol-based polyether, 20 parts of inositol phosphate-based polyether, 8 parts of alcohol adjuvant, and 42 parts of water; or The pesticide synergist, by weight, comprises: 40 parts of silanol-based polyether, 10 parts of inositol phosphate-based polyether, 10 parts of alcohol adjuvant, and 40 parts of water; or The pesticide synergist, by weight, comprises: 10 parts of silanol-based polyether, 30 parts of inositol phosphate-based polyether, 6 parts of alcohol adjuvant, and 54 parts of water.

7. The pesticide synergist according to any one of claims 1-4, characterized in that, The silanol-based polyether is prepared by the following method: Using silanol as an initiator, an addition reaction is carried out with epoxide alkane in the presence of a basic catalyst to complete etherification; Optionally, the alkaline catalyst is selected from sodium hydroxide, lithium hydroxide, or potassium hydroxide, preferably potassium hydroxide; the amount of the alkaline catalyst is 0.1% to 1% of the total mass of the reaction raw materials, preferably 0.3% to 0.5%; and / or The silanol is selected from one or more combinations of trimethylsilanol, triethylsilanol, tripropylsilanol, tributylsilanol, and triphenylsilanol, preferably one or a combination of trimethylsilanol and triethylsilanol, and more preferably triethylsilanol; and / or The epoxide is selected from one or more combinations of ethylene oxide, propylene oxide, and butane; optionally, the molar ratio of the silanol, propylene oxide, ethylene oxide, and butane is 1 : (0 to 100) : (1 to 200) : (0 to 50); and / or The epoxide is one or a combination of ethylene oxide and propylene oxide; optionally, the molar ratio of the silanol, propylene oxide and ethylene oxide is 1:(0 to 100):(1 to 200); and / or The addition reaction is performed at a temperature of 80°C to 150°C, preferably 120°C to 130°C. The reaction time for the addition reaction is 2 to 8 hours, preferably 4 to 6 hours.

8. The pesticide synergist according to any one of claims 1-4, characterized in that, The inositol phosphate-based polyether is prepared by the following method: Using one or more of inositol phosphate esters as initiators, an addition reaction is carried out with epoxide alkane in the presence of a basic catalyst to complete etherification; Optionally, the alkaline catalyst is selected from sodium hydroxide, lithium hydroxide, or potassium hydroxide, preferably potassium hydroxide; the amount of the alkaline catalyst is 0.1% to 1% of the total mass of the reaction raw materials, preferably 0.3% to 0.5%; and / or The inositol phosphate is selected from at least one or more combinations of inositol diphosphate, inositol triphosphate, inositol tetraphosphate, inositol pentphosphate, and inositol hexaphosphate; and / or The epoxide is selected from at least one or more combinations of ethylene oxide, propylene oxide, and butane; optionally, the molar ratio of inositol phosphate, propylene oxide, ethylene oxide, and butane is 1 : (0 to 50) : (1 to 100) : (0 to 50); and / or The alkyl oxide is one or a combination of ethylene oxide and propylene oxide; optionally, the molar ratio of inositol phosphate, propylene oxide and ethylene oxide is 1:(0 to 50):(1 to 100), or optionally 1:(10 to 40):(10 to 50); and / or The addition reaction is carried out at a temperature of 80°C to 150°C, preferably 120°C to 130°C; and / or The addition reaction takes 2 to 8 hours, preferably 4 to 6 hours.

9. The pesticide synergist according to any one of claims 1-4, characterized in that, The alcohol additive is selected from at least one of methanol, ethanol, propanol, butanol, ethylene glycol, propylene glycol, and glycerol, preferably propylene glycol or glycerol.

10. A method for preparing the pesticide synergist according to claims 1-9, comprising: The polyether is prepared by mixing silanol-based polyether, inositol phosphate-based polyether, alcohol additives, and water. Optionally, the mixing is performed by stirring at 25°C to 40°C for 40 min to 60 min.

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