WO2021093266A1 - Compound insecticidal and acaricidal nano aqueous formulation containing lambda-cyhalothrin and emamectin benzoate, and use thereof - Google Patents

Compound insecticidal and acaricidal nano aqueous formulation containing lambda-cyhalothrin and emamectin benzoate, and use thereof Download PDF

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WO2021093266A1
WO2021093266A1 PCT/CN2020/085514 CN2020085514W WO2021093266A1 WO 2021093266 A1 WO2021093266 A1 WO 2021093266A1 CN 2020085514 W CN2020085514 W CN 2020085514W WO 2021093266 A1 WO2021093266 A1 WO 2021093266A1
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cyhalothrin
lambda
nano
emamectin benzoate
aqueous agent
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PCT/CN2020/085514
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French (fr)
Chinese (zh)
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白杰
邢刚
陈叶青
杨琴
郭崇友
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南京华洲药业有限公司
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    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N25/00Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
    • A01N25/02Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing liquids as carriers, diluents or solvents
    • A01N25/04Dispersions, emulsions, suspoemulsions, suspension concentrates or gels
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N43/00Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/90Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having two or more relevant hetero rings, condensed among themselves or with a common carbocyclic ring system
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N53/00Biocides, pest repellants or attractants, or plant growth regulators containing cyclopropane carboxylic acids or derivatives thereof

Definitions

  • the invention belongs to the field of pesticides, and relates to an insecticidal and acaricidal nano-aqueous agent with lambda-cyhalothrin and emamectin benzoate as main effective ingredients and uses thereof.
  • Lambda-cyhalothrin (lambda-cyhalothrin), molecular formula: C 23 H 19 ClF 3 NO 3 .
  • Emamectin Benzoate molecular formula: C 56 H 81 NO 15 .
  • Chemical name: 4'-epi-methylamino-4'-deoxyabamectin B1 benzoate, Chinese alias: emamectin salt, is a new type of high-efficiency semi-synthesis synthesized from the fermentation product of abamectin B1 Antibiotic insecticide, it has the characteristics of super high efficiency, low toxicity (nearly non-toxic preparation), low residue, no pollution and other biological pesticides. It is widely used for the prevention and control of various pests on vegetables, fruit trees, cotton and other crops.
  • Insecticides containing a single ingredient often have shortcomings in the prevention and control of pesticide pests: continuous use is prone to pesticide resistance, narrow insecticidal spectrum, cannot provide comprehensive protection for crops, and high pesticide costs for farmers.
  • the combination of two or more active ingredients with synergistic effect can improve the control effect, reduce the dosage of active ingredients, save costs, slow down the occurrence of pests and mite resistance, and expand the control spectrum. Insects can be cured at the same time, reducing the use cost of farmers.
  • the conventional dosage forms of lambda-cyhalothrin and emamectin benzoate are mainly emulsifiable concentrates, which contain a large amount of organic solvents, which pose safety hazards in production and cause serious harm to the environment in field use. Reducing the use of organic solvents and developing aqueous formulations is the inevitable way for the development of lambda-cyhalothrin and emamectin benzoate formulations.
  • the purpose of the present invention is to provide a composite insecticidal and acaricidal nano-aqueous agent containing lambda-cyhalothrin and emamectin benzoate (emamectin salt).
  • the nano-aqueous agent contains lambda-cyhalothrin
  • the compound of pyrethroid and emamectin benzoate has obvious synergistic effect.
  • nano-scale micelles formed by the active agent carry lambda-cyhalothrin and emamectin benzoate that are insoluble in water, and the active ingredients are present in the nano-aqueous agent as nano-scale particles, which is more convenient for its adhesion, spreading and penetration on the target. It is more resistant to rain washing, and does not contain organic solvents, which is safe and environmentally friendly.
  • the nano-aqueous agent contains the following ingredients: Lambda-cyhalothrin and Emamectin benzoate.
  • the total percentage content is 3-50%, the weight percentage of the surfactant is 5-20%, and the balance is water.
  • the weight ratio of the lambda-cyhalothrin and emamectin benzoate is 20:1 to 1:20, preferably 1:5 to 5:1.
  • the total weight percentage content of the nano-aqueous lambda-cyhalothrin and emamectin benzoate in the composite insecticidal composition is preferably 3%-21%.
  • the nano-aqueous agent of the present invention can only contain the active ingredients lambda cyhalothrin and emamectin benzoate, and other components can also be added to the active ingredients during use or preparation.
  • the effective ingredients of the acaricidal nano-aqueous agent can also be present in the composition in a synergistic effective amount.
  • Said surfactant is selected from fatty alcohol polyoxyethylene ether, alkylphenol formaldehyde resin polyoxyethylene ether, styrylphenol polyoxyethylene ether, fatty alcohol polyoxyethylene ether phosphate, tristyrylphenol polyoxyethylene
  • fatty alcohol polyoxyethylene ether alkylphenol formaldehyde resin polyoxyethylene ether
  • styrylphenol polyoxyethylene ether fatty alcohol polyoxyethylene ether phosphate
  • tristyrylphenol polyoxyethylene One or more combinations of vinyl ether phosphate, alkylphenol polyoxyethylene ether phosphate, sodium alcohol ether succinate monoester sulfonate, sorbitan fatty acid ester polyoxyethylene ether, and the like.
  • Another object of the present invention is to provide a method for preparing a nano-aqueous agent containing lambda-cyhalothrin and emamectin benzoate, which includes:
  • Step (1) at room temperature (10 ⁇ 35 °C), the lambda-cyhalothrin technical medicine, emamectin benzoate technical medicine and surfactant are mixed, stirred to make Lambda cyanofluoride Pyrethrin and emamectin benzoate are uniformly dispersed in the surfactant;
  • Step (2) Add water under stirring and stir evenly to form a surfactant micellar solution containing lambda-cyhalothrin and emamectin benzoate, which is a transparent lambda-chlorofluorocyanate Pyrethrin and emamectin benzoate nano-aqueous agent.
  • the high-efficiency cyhalothrin and emamectin benzoate nano-aqueous agent of the present invention has a transparent appearance, and the average particle size of surfactant micelles is nanometer level; after entering water, it can quickly dissolve with water to form a completely transparent solution.
  • the dilution stability is qualified; the nano-aqueous agent of the present invention has stable performance, and is still stable after cold storage at 0°C for 7 days and hot storage at 54°C for 14 days, lambda-cyhalothrin will not precipitate, and storage is convenient.
  • step (1) the stirring speed is 60-100 revolutions per second, and the stirring time is 0.5h.
  • the technician can adjust the time to make the lambda-cyhalothrin and emamectin benzoate uniformly dispersed in The surface active agent shall prevail.
  • step (2) the stirring speed is 60-100 revolutions per second, and the stirring is continued for 0.5-1 h after adding water.
  • Another object of the present invention is to provide the use of the nano-aqueous agent for controlling pests and harmful mites on fruit trees, cotton and vegetables.
  • the pest is cotton bollworm
  • the pest mite is cotton spider mite
  • the nano-aqueous agent of the present invention can reduce the amount used, delay the generation of insect pests and mite resistance, and can also improve the control effect, which is better than single-agent use, saves time and effort, saves costs, reduces environmental pollution, and reduces farmers burden.
  • the compound has obvious synergistic effect, which improves the control effect of pests and harmful mites compared with single use alone;
  • the present invention is a new dosage form-nano-aqueous agent, which has a nanometer particle size, is more convenient for its attachment, spreading and penetration on the target, is more resistant to rain washing, does not contain organic solvents, and is safe and environmentally friendly.
  • Figure 1 shows the 11% lambda-cyhalothrin ⁇ emamectin benzoate nano-aqueous agent of Example 2.
  • Figure 2 shows the 11% beta-cyhalothrin ⁇ emamectin benzoate unqualified water formulation of Comparative Example 4.
  • Single-dose toxicity index standard drug LC50/a single-dose LC50 ⁇ 100
  • Toxicity Index A single dose toxicity index ⁇ A single dose proportion in the mixture + B single dose toxicity index ⁇ B single dose proportion in the mixture
  • ATI Measured Toxicity Index
  • CTC measured toxicity index of the mixture (ATI)/theoretical toxicity index of the mixture (TTI) ⁇ 100
  • Co-toxicity coefficient classification when CTC is greater than 120, the mixture has synergistic effect, when CTC is less than 80, it is antagonistic, and CTC between 80-120 is additive.
  • the ratio of lambda-cyhalothrin and emamectin benzoate ranges from 20:1 to 1:20, and the co-toxicity coefficient is greater than 120, which is effective in the prevention and control of cotton spider mites.
  • the synergistic effect especially between 5:1 and 1:5, the co-toxicity coefficient is above 160, and the synergistic effect is significant.
  • the ratio of lambda-cyhalothrin and emamectin benzoate ranges from 20:1 to 1:20, and the co-toxicity coefficient is greater than 120, which has a synergistic effect on the control of Plutella xylostella The effect, especially between 5:1 and 1:5, the co-toxicity coefficient is above 180, and the synergistic effect is significant.
  • Preparation method At room temperature (10 ⁇ 35°C), weigh 20g (based on active ingredients, the same below) lambda-cyhalothrin technical and 1g (based on active ingredients, the same below) emamectin benzene
  • the formate is mixed with 5g styrene phenol polyoxyethylene ether, 11g alkylphenol polyoxyethylene ether phosphate, 6g fatty alcohol polyoxyethylene ether phosphate, stir at 90 rpm for 0.5h, keep stirring, add 57g water, continue to stir for 0.5h to obtain 21% lambda-cyhalothrin ⁇ emamectin benzoate nano-aqueous agent.
  • the nano-aqueous agent of this example has a slightly yellow appearance, a viscosity of 152 mPa ⁇ s, and an average particle size of 15.6 nanometers.
  • the nano-aqueous agent of this embodiment can quickly dissolve with water to form a completely transparent solution, and the dilution stability is qualified.
  • the preparation method is the same as that in Example 1, and 11% lambda-cyhalothrin ⁇ emamectin benzoate nano-aqueous agent is prepared.
  • the nano-aqueous agent of this example has a transparent and slightly yellowish appearance, a viscosity of 105 mPa ⁇ s, and an average particle size of 15.0 nanometers.
  • the nano-aqueous agent of this embodiment can quickly dissolve with water to form a completely transparent solution, and the dilution stability is qualified.
  • the preparation method is the same as in Example 1, and 6% lambda-cyhalothrin ⁇ emamectin benzoate nano-aqueous agent is prepared.
  • the nano-aqueous agent of this example has a transparent and slightly yellow appearance, a viscosity of 100 mPa ⁇ s, and an average particle size of 13.5 nanometers.
  • the nano-aqueous agent of this embodiment can quickly dissolve with water to form a completely transparent solution, and the dilution stability is qualified.
  • the preparation method is the same as that in Example 1, and a 3% lambda-cyhalothrin ⁇ emamectin benzoate nano-aqueous agent is prepared.
  • the nano-aqueous agent of this example has a transparent and slightly yellowish appearance, a viscosity of 85.5 mPa ⁇ s, and an average particle size of 17.5 nanometers.
  • the nano-aqueous agent of this embodiment can quickly dissolve with water to form a completely transparent solution, and the dilution stability is qualified.
  • the preparation method is the same as that in Example 1, and a 4% lambda-cyhalothrin ⁇ aminoabamectin benzoate nano-water formulation is prepared.
  • the nano-aqueous agent of this example has a transparent and slightly yellowish appearance, a viscosity of 95 mPa ⁇ s, and an average particle size of 13 nanometers.
  • the nano-aqueous agent of this embodiment can quickly dissolve with water to form a completely transparent solution, and the dilution stability is qualified.
  • the preparation method is the same as that in Example 1, and 9% lambda-cyhalothrin ⁇ emamectin benzoate nano-aqueous agent is prepared.
  • the nano-aqueous agent of this example has a transparent and slightly yellowish appearance, a viscosity of 92 mPa ⁇ s, and an average particle size of 15.5 nanometers.
  • the nano-aqueous agent of this embodiment can quickly dissolve with water to form a completely transparent solution, and the dilution stability is qualified.
  • the preparation method is the same as that of Example 1, and 12% lambda-cyhalothrin ⁇ emamectin benzoate nano-aqueous agent is prepared.
  • the nano-aqueous agent of this example has a transparent and slightly yellowish appearance, a viscosity of 98 mPa ⁇ s, and an average particle size of 14.7 nanometers.
  • the nano-aqueous agent of this embodiment can quickly dissolve with water to form a completely transparent solution, and the dilution stability is qualified.
  • the preparation method is the same as that in Example 1, and 11% lambda-cyhalothrin ⁇ emamectin benzoate nano-aqueous agent is prepared.
  • the nano-aqueous agent of this embodiment has a transparent and slightly yellowish appearance, a viscosity of 105 mPa ⁇ s, and an average particle size of 18.6 nanometers.
  • the nano-aqueous agent of this embodiment can quickly dissolve with water to form a completely transparent solution, and the dilution stability is qualified.
  • the preparation method is the same as that in Example 1, and 10.5% lambda-cyhalothrin ⁇ emamectin benzoate nano-aqueous agent was prepared.
  • the nano-aqueous agent of this example has a transparent and slightly yellowish appearance, a viscosity of 102 mPa ⁇ s, and an average particle size of 15.5 nanometers.
  • the nano-aqueous agent of this embodiment can quickly dissolve with water to form a completely transparent solution, and the dilution stability is qualified.
  • the water preparation is prepared with the commonly used auxiliary (wetting agent) in the preparation of water preparation, and the specific formula is shown in Table 3.
  • the preparation method is the same as in Example 1.
  • an aqueous solution can be prepared at room temperature (10 ⁇ 35°C), but the aqueous solution is placed at low temperature (below 0°C), lambda-cyhalothrin and emamectin
  • the original benzoic acid salt will continue to precipitate out, and it cannot be recovered after the temperature rises. It shows that the use of surfactants other than the surfactants of the present invention or conventional water agents other than the surfactant composition cannot be used to prepare qualified lambda cyhalothrin ⁇ aminoabamectin benzoate nano Water agent.
  • Test agent Example 1 to Example 9 Lambda-cyhalothrin ⁇ Emmamectin benzoate compound nano-aqueous agent.
  • Control object cotton spider mite.
  • Test method The normal field dosage (active ingredient) was used, the dosage treatment was set for three repetitions, and the random block arrangement was repeated, and the area of each repetition was 30m 2.
  • the experiment used a knapsack sprayer to spray the whole cotton. Investigate the number of insect populations before application, and investigate the number of remaining live insects 3 days, 7 days, 14 days, and 30 days after application, and calculate the control effect according to the following method:
  • Insect population reduction rate (%) (number of insects before application-number of insects after application) / number of insects before application ⁇ 100
  • Corrected control effect (%) (Reduction rate of insect population in the treatment area-Reduction rate of insect population in the control area) / (100-Recession rate of insect population in the control area before and after control) ⁇ 100
  • Table 4 Field test results of Lambda-cyhalothrin-Avermectin benzoate paired with cotton spider mite
  • Test agent Example 1 to Example 9 Lambda-cyhalothrin ⁇ Emmamectin benzoate compound nano-aqueous agent.
  • Control object Plutella xylostella.
  • Test method The normal field dosage (active ingredient) was used, the dosage treatment was set for three repetitions, and the random block arrangement was repeated, and the area of each repetition was 50m 2.
  • the experiment used a knapsack sprayer to spray the whole cotton. Investigate the number of insect populations before application, and investigate the number of remaining live insects 3 days, 7 days, 14 days, and 30 days after application, and calculate the control effect according to the following method:
  • Insect population reduction rate (%) (number of insects before application-number of insects after application) / number of insects before application ⁇ 100
  • Corrected control effect (%) (Reduction rate of insect population in the treatment area-Reduction rate of insect population in the control area) / (100-Recession rate of insect population in the control area before and after control) ⁇ 100
  • Table 5 Field test results of Lambda-cyhalothrin-Avermectin benzoate paired with Plutella xylostella

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Abstract

Disclosed in the present invention is a compound insecticidal and acaricidal nano aqueous formulation containing lambda-cyhalothrin and emamectin benzoate, having lambda-cyhalothrin and emamectin benzoate as active ingredients, and formed by compounding with a surfactant and water. The mass percentage of the lambda-cyhalothrin and the emamectin benzoate is 3-50%, that of the surfactant is 5-20%, and the remainder is water. The mass ratio between the lambda-cyhalothrin and the emamectin benzoate is 20:1 - 1:20. In the present invention, nano-sized micelles formed by the surfactant are used to carry poorly water-soluble lambda-cyhalothrin and emamectin benzoate, such that the two active ingredients exist in the nano aqueous formulation as nano-sized microparticles, which facilitates the adhesion, spreading, and penetration of the active ingredients onto, over, and into a target, and increases the resistance of the active ingredients to rain wash. With the two active ingredients acting in synergy, the nano aqueous formulation can prevent and treat Lepidoptera and mite pests on agricultural crops with both a fast pesticidal effect and a prolonged efficacy, providing markedly superior prevention and treatment performances to those achieved by separate use of the two ingredients.

Description

含高效氯氟氰菊酯和甲氨基阿维菌素苯甲酸盐的复合杀虫杀螨纳米水剂及其用途Composite insecticidal and acaricidal nano water agent containing lambda-cyhalothrin and emamectin benzoate and its use 技术领域Technical field
本发明属于农药领域,涉及一种以高效氯氟氰菊酯和甲氨基阿维菌素苯甲酸盐为主要有效成分的杀虫杀螨纳米水剂及其用途。The invention belongs to the field of pesticides, and relates to an insecticidal and acaricidal nano-aqueous agent with lambda-cyhalothrin and emamectin benzoate as main effective ingredients and uses thereof.
背景技术Background technique
高效氯氟氰菊酯(lambda-cyhalothrin),分子式:C 23H 19ClF 3NO 3。化学名称:3-(2-氯-3,3,3-三氟丙烯基)-2,2-二甲基环丙烷羧酸α-氰基-3-苯氧苄基酯。是一种高效、广谱、速效拟除虫菊酯类杀虫、杀螨剂,以触杀和胃毒作用为主,无内吸作用。对鳞翅目、鞘翅目和半翅目等多种害虫和其他害虫,以及叶螨、锈螨、瘿螨等有良好效果,在虫、螨并发时可以兼治,可防治棉红铃虫和棉铃虫、菜青虫、菜缢管蚜、茶尺蠖、茶毛虫、茶橙瘿螨、叶瘿螨、柑橘叶蛾、橘蚜以及柑橘叶螨、锈螨、桃小食心虫及梨小食心虫等,也可用来防治多种地表和公共卫生害虫。 Lambda-cyhalothrin (lambda-cyhalothrin), molecular formula: C 23 H 19 ClF 3 NO 3 . Chemical name: 3-(2-Chloro-3,3,3-trifluoropropenyl)-2,2-dimethylcyclopropanecarboxylic acid α-cyano-3-phenoxybenzyl ester. It is a highly effective, broad-spectrum, quick-acting pyrethroid insecticide and acaricide, mainly for contact and stomach toxicity, without systemic effects. It has a good effect on Lepidoptera, Coleoptera and Hemiptera and other pests and other pests, as well as spider mites, rust mites, and gall mites. It can treat both insects and mites concurrently, and can prevent cotton bollworms and cotton bolls. Insects, cabbage caterpillars, pipe aphid, tea looper, tea caterpillars, tea orange gall mites, leaf gall mites, citrus leaf moths, orange aphid and citrus spider mites, rust mites, peach heartworm and pear heartworm, etc., can also be used to control A variety of surface and public health pests.
甲氨基阿维菌素苯甲酸盐(Emamectin Benzoate),分子式:C 56H 81NO 15。化学名称:4'-表-甲氨基-4'-脱氧阿维菌素B1苯甲酸盐,中文别名:甲维盐,是从发酵产品阿维菌素B1开始合成的一种新型高效半合成抗生素杀虫剂,它具有超高效、低毒(制剂近无毒)、低残留、无公害等生物农药的特点。广泛用于蔬菜、果树、棉花等农作物上的多种害虫的防治。 Emamectin Benzoate, molecular formula: C 56 H 81 NO 15 . Chemical name: 4'-epi-methylamino-4'-deoxyabamectin B1 benzoate, Chinese alias: emamectin salt, is a new type of high-efficiency semi-synthesis synthesized from the fermentation product of abamectin B1 Antibiotic insecticide, it has the characteristics of super high efficiency, low toxicity (nearly non-toxic preparation), low residue, no pollution and other biological pesticides. It is widely used for the prevention and control of various pests on vegetables, fruit trees, cotton and other crops.
含单一成分的杀虫剂品种在农药害虫防治中往往存在缺陷:连续使用容易产生抗药性,杀虫谱窄,不能为作物提供全面的保护,农民用药成本高等。具有增效作用的两种或者两种以上活性成分的组合混配,可以提高防效,减少有效成分地用药量,节约成本,减缓害虫害螨抗性发生、并能扩大防治谱,起到多虫兼治,降低农民的使用成本。Insecticides containing a single ingredient often have shortcomings in the prevention and control of pesticide pests: continuous use is prone to pesticide resistance, narrow insecticidal spectrum, cannot provide comprehensive protection for crops, and high pesticide costs for farmers. The combination of two or more active ingredients with synergistic effect can improve the control effect, reduce the dosage of active ingredients, save costs, slow down the occurrence of pests and mite resistance, and expand the control spectrum. Insects can be cured at the same time, reducing the use cost of farmers.
目前,高效氯氟氰菊酯、甲氨基阿维菌素苯甲酸盐的常规剂型主要为乳油,其中含有大量有机溶剂,在生产中存在安全隐患,田间使用中会对环境造成严重危害。减少有机溶剂的使用,发展水剂剂型,是高效氯氟氰菊酯、甲氨基阿维菌素苯甲酸盐剂型发展必然之路。At present, the conventional dosage forms of lambda-cyhalothrin and emamectin benzoate are mainly emulsifiable concentrates, which contain a large amount of organic solvents, which pose safety hazards in production and cause serious harm to the environment in field use. Reducing the use of organic solvents and developing aqueous formulations is the inevitable way for the development of lambda-cyhalothrin and emamectin benzoate formulations.
发明内容Summary of the invention
本发明的目的是提供一种含高效氯氟氰菊酯和甲氨基阿维菌素苯甲酸盐(甲维盐)的复合杀虫杀螨纳米水剂,该纳米水剂中高效氯氟氰菊酯和甲维盐复配具有明显的协同增效作用,另外,创造性的发现某些表面活性剂,采用表面活性剂胶束增溶技术,在不使用有机溶剂助溶的情况下,利用表面活性剂形成的纳米级胶束承载难溶于水的高效氯氟氰菊酯和甲维盐,有效成 分以纳米级微粒存在于纳米水剂中,更便于其在靶标上附着展布和渗透,更耐雨水冲刷,且不含有机溶剂,安全环保。The purpose of the present invention is to provide a composite insecticidal and acaricidal nano-aqueous agent containing lambda-cyhalothrin and emamectin benzoate (emamectin salt). The nano-aqueous agent contains lambda-cyhalothrin The compound of pyrethroid and emamectin benzoate has obvious synergistic effect. In addition, some surfactants were creatively discovered, using surfactant micellar solubilization technology, and the use of surface The nano-scale micelles formed by the active agent carry lambda-cyhalothrin and emamectin benzoate that are insoluble in water, and the active ingredients are present in the nano-aqueous agent as nano-scale particles, which is more convenient for its adhesion, spreading and penetration on the target. It is more resistant to rain washing, and does not contain organic solvents, which is safe and environmentally friendly.
本发明的目的是通过以下技术方案实现的:The purpose of the present invention is achieved through the following technical solutions:
一种含高效氯氟氰菊酯和甲氨基阿维菌素苯甲酸盐的复合杀虫杀螨纳米水剂,所述的纳米水剂以高效氯氟氰菊酯和甲氨基阿维菌素苯甲酸盐为主要活性成分,与表面活性剂和水配制而成,其中,所述的纳米水剂含有以下成分:高效氯氟氰菊酯和甲氨基阿维菌素苯甲酸盐的重量百分含量总和为3~50%,表面活性剂的重量百分含量为5~20%,余量为水。A composite insecticidal and acaricidal nano-aqueous agent containing lambda-cyhalothrin and emamectin benzoate, wherein the nano-aqueous agent contains lambda-cyhalothrin and emamectin Benzoate is the main active ingredient and is formulated with surfactant and water. The nano-aqueous agent contains the following ingredients: Lambda-cyhalothrin and Emamectin benzoate. The total percentage content is 3-50%, the weight percentage of the surfactant is 5-20%, and the balance is water.
所述的高效氯氟氰菊酯和甲氨基阿维菌素苯甲酸盐的重量比为20:1-1:20,优选为1:5-5:1。The weight ratio of the lambda-cyhalothrin and emamectin benzoate is 20:1 to 1:20, preferably 1:5 to 5:1.
所述的纳米水剂高效氯氟氰菊酯与甲氨基阿维菌素苯甲酸盐二者在该复合杀虫组合物中的重量百分含量总和优选为3%~21%。The total weight percentage content of the nano-aqueous lambda-cyhalothrin and emamectin benzoate in the composite insecticidal composition is preferably 3%-21%.
本发明所述的纳米水剂可以只含有活性成分高效氯氟氰菊酯和甲氨基阿维菌素苯甲酸盐,也可在使用或配制时向活性成分中加入其他组分,该杀虫杀螨纳米水剂的有效成份还可以增效有效量存在于组合物中。The nano-aqueous agent of the present invention can only contain the active ingredients lambda cyhalothrin and emamectin benzoate, and other components can also be added to the active ingredients during use or preparation. The effective ingredients of the acaricidal nano-aqueous agent can also be present in the composition in a synergistic effective amount.
所述的表面活性剂选自脂肪醇聚氧乙烯醚、烷基酚甲醛树脂聚氧乙烯醚、苯乙烯基苯酚聚氧乙烯醚、脂肪醇聚氧乙烯醚磷酸酯、三苯乙烯基苯酚聚氧乙烯醚磷酸酯、烷基酚聚氧乙烯醚磷酸酯、醇醚琥珀酸单酯磺酸钠、失水山梨醇脂肪酸酯聚氧乙烯醚等中的一种或多种组合。Said surfactant is selected from fatty alcohol polyoxyethylene ether, alkylphenol formaldehyde resin polyoxyethylene ether, styrylphenol polyoxyethylene ether, fatty alcohol polyoxyethylene ether phosphate, tristyrylphenol polyoxyethylene One or more combinations of vinyl ether phosphate, alkylphenol polyoxyethylene ether phosphate, sodium alcohol ether succinate monoester sulfonate, sorbitan fatty acid ester polyoxyethylene ether, and the like.
本发明的另一个目的是提供一种含高效氯氟氰菊酯和甲氨基阿维菌素苯甲酸盐的纳米水剂的制备方法,包括:Another object of the present invention is to provide a method for preparing a nano-aqueous agent containing lambda-cyhalothrin and emamectin benzoate, which includes:
步骤(1)、在常温(10~35℃)下,将高效氯氟氰菊酯原药、甲氨基阿维菌素苯甲酸盐原药与表面活性剂混合,搅拌,使高效氯氟氰菊酯和甲氨基阿维菌素苯甲酸盐均匀分散在表面活性剂中;Step (1), at room temperature (10 ~ 35 ℃), the lambda-cyhalothrin technical medicine, emamectin benzoate technical medicine and surfactant are mixed, stirred to make Lambda cyanofluoride Pyrethrin and emamectin benzoate are uniformly dispersed in the surfactant;
步骤(2)、在搅拌状态下加入水,搅拌均匀,形成含有高效氯氟氰菊酯和甲氨基阿维菌素苯甲酸盐的表面活性剂胶束溶液,即为透明的高效氯氟氰菊酯和甲氨基阿维菌素苯甲酸盐纳米水剂。Step (2). Add water under stirring and stir evenly to form a surfactant micellar solution containing lambda-cyhalothrin and emamectin benzoate, which is a transparent lambda-chlorofluorocyanate Pyrethrin and emamectin benzoate nano-aqueous agent.
本发明高效氯氟氰菊酯和甲氨基阿维菌素苯甲酸盐纳米水剂外观透明,表面活性剂胶束平均粒径为纳米级别;入水后能迅速与水互溶,形成完全透明溶液,稀释稳定性合格;本发明纳米水剂性能稳定,在0℃冷贮7d和54℃热贮14d后仍然稳定,高效氯氟氰菊酯不会析出,便于贮藏。The high-efficiency cyhalothrin and emamectin benzoate nano-aqueous agent of the present invention has a transparent appearance, and the average particle size of surfactant micelles is nanometer level; after entering water, it can quickly dissolve with water to form a completely transparent solution. The dilution stability is qualified; the nano-aqueous agent of the present invention has stable performance, and is still stable after cold storage at 0°C for 7 days and hot storage at 54°C for 14 days, lambda-cyhalothrin will not precipitate, and storage is convenient.
步骤(1)中,搅拌速度为60~100转/秒,搅拌时间为0.5h,技术人员可以调整时间,以使 高效氯氟氰菊酯和甲氨基阿维菌素苯甲酸盐均匀分散在表面活性剂中为准。In step (1), the stirring speed is 60-100 revolutions per second, and the stirring time is 0.5h. The technician can adjust the time to make the lambda-cyhalothrin and emamectin benzoate uniformly dispersed in The surface active agent shall prevail.
步骤(2)中,搅拌速度为60~100转/秒,加入水之后继续搅拌0.5~1h。In step (2), the stirring speed is 60-100 revolutions per second, and the stirring is continued for 0.5-1 h after adding water.
本发明的另一目的是提供所述的纳米水剂在防治果树、棉花、蔬菜上的害虫、害螨的用途。Another object of the present invention is to provide the use of the nano-aqueous agent for controlling pests and harmful mites on fruit trees, cotton and vegetables.
进一步的,所述的害虫为棉铃虫,所述的害螨为棉红蜘蛛。Further, the pest is cotton bollworm, and the pest mite is cotton spider mite.
本发明纳米水剂在使用过程中,可以减少使用量,延缓害虫害螨抗药性的产生,还能提高防治效果,优于单剂使用,省时省力、节约成本及减少对环境的污染,减轻农民负担。During use, the nano-aqueous agent of the present invention can reduce the amount used, delay the generation of insect pests and mite resistance, and can also improve the control effect, which is better than single-agent use, saves time and effort, saves costs, reduces environmental pollution, and reduces Farmers burden.
与现有技术相比本发明的有益效果:Compared with the prior art, the beneficial effects of the present invention:
(1)复配具有明显的协同增效作用,较之单剂单独使用,提高了对害虫、害螨的防治效果;(1) The compound has obvious synergistic effect, which improves the control effect of pests and harmful mites compared with single use alone;
(2)兼有速效和长效;(2) Both quick-acting and long-acting;
(3)两种有效成分复配降低了农药使用量,降低了生产和使用成本及对环境的污染;(3) The combination of two active ingredients reduces the amount of pesticides used, reduces production and use costs and environmental pollution;
(4)延缓害虫、害螨对农药的抗性,其效果明显高于其单剂使用;(4) Delay the resistance of pests and mites to pesticides, and its effect is significantly higher than its single-dose use;
(5)本发明为全新剂型-纳米水剂,具有纳米级粒径大小,更便于其在靶标上附着、展布和渗透,更耐雨水冲刷,且不含有有机溶剂,安全环保。(5) The present invention is a new dosage form-nano-aqueous agent, which has a nanometer particle size, is more convenient for its attachment, spreading and penetration on the target, is more resistant to rain washing, does not contain organic solvents, and is safe and environmentally friendly.
附图说明Description of the drawings
图1为实施例2的11%的高效氯氟氰菊酯·甲维盐纳米水剂。Figure 1 shows the 11% lambda-cyhalothrin·emamectin benzoate nano-aqueous agent of Example 2.
图2为对比例4的11%的高效氯氟氢菊酯·甲维盐不合格水剂。Figure 2 shows the 11% beta-cyhalothrin·emamectin benzoate unqualified water formulation of Comparative Example 4.
具体实施方式Detailed ways
以下结合实施例对本发明作进一步说明,但不以任何方式限制本发明。The present invention will be further described in conjunction with the following examples, but the present invention will not be restricted in any way.
室内毒力测定Indoor toxicity test
1、采用浸渍玻片法进行高效氯氟氰菊酯和甲氨基阿维菌素苯甲酸盐及其复配样品对棉红蜘蛛的毒力测定,每处理重复3次,每浓度处理30头,用LC 50值依据孙云沛法计算共毒系数(CTC值): 1. The virulence of lambda-cyhalothrin and emamectin benzoate and their mixed samples to the cotton spider mites were determined by the dip-slide method. Each treatment was repeated 3 times, and each concentration was treated with 30 heads. , Use LC 50 value to calculate co-toxicity coefficient (CTC value) according to Sun Yunpei's method:
单剂毒力指数=标准药剂LC50/某单剂LC50×100Single-dose toxicity index = standard drug LC50/a single-dose LC50×100
理论毒力指数(TTI)=A单剂的毒力指数×A单剂在混剂中所占比例+B单剂的毒力指数×B单剂在混剂中所占比例Theoretical Toxicity Index (TTI) = A single dose toxicity index × A single dose proportion in the mixture + B single dose toxicity index × B single dose proportion in the mixture
实测毒力指数(ATI)=标准单剂的LC50值/混剂的LC50值×100Measured Toxicity Index (ATI) = LC50 value of standard single agent/LC50 value of mixed agent×100
共毒系数(CTC)=混剂实测毒力指数(ATI)/混剂理论毒力指数(TTI)×100Co-toxicity coefficient (CTC) = measured toxicity index of the mixture (ATI)/theoretical toxicity index of the mixture (TTI) × 100
共毒系数分级:CTC大于120时混剂具有协同增效性,CTC小于80时为拮抗,CTC在80-120之间为相加作用。Co-toxicity coefficient classification: when CTC is greater than 120, the mixture has synergistic effect, when CTC is less than 80, it is antagonistic, and CTC between 80-120 is additive.
结果见表1。The results are shown in Table 1.
表1高效氯氟氰菊酯和甲氨基阿维菌素苯甲酸盐复配对棉红蜘蛛的室内毒力测定Table 1 Indoor Toxicity Determination of Lambda-cyhalothrin and Emamectin Benzoate on Cotton Red Spider
Figure PCTCN2020085514-appb-000001
Figure PCTCN2020085514-appb-000001
由表1可知,高效氯氟氰菊酯和甲氨基阿维菌素苯甲酸盐配比范围在20:1-1:20之间,共毒系数都大于120,对棉红蜘蛛的防治具有增效作用,尤其在5:1-1:5之间,共毒系数在160以上,增效作用显著。It can be seen from Table 1 that the ratio of lambda-cyhalothrin and emamectin benzoate ranges from 20:1 to 1:20, and the co-toxicity coefficient is greater than 120, which is effective in the prevention and control of cotton spider mites. The synergistic effect, especially between 5:1 and 1:5, the co-toxicity coefficient is above 160, and the synergistic effect is significant.
2、采用饲料混毒法,选择青菜小菜蛾为目标害虫,每处理重复三次,用几率值法计算各药剂对青菜小菜蛾的毒力回归方程和致死中浓度LC 50,用LC 50值按照孙云沛法计算共度系数,结果如表2: 2. Using the feed mixing method, select Plutella xylostella as the target pest, and repeat each treatment three times. Use the probability value method to calculate the virulence regression equation of each agent against Plutella xylostella and the lethal concentration LC 50 , and use the LC 50 value according to Sun Yunpei Method to calculate the co-degree coefficient, the results are shown in Table 2:
表2高效氯氟氰菊酯和甲氨基阿维菌素苯甲酸盐复配对小菜蛾的毒力测定Table 2 Toxicity determination of the combination of lambda-cyhalothrin and emamectin benzoate in Plutella xylostella
Figure PCTCN2020085514-appb-000002
Figure PCTCN2020085514-appb-000002
Figure PCTCN2020085514-appb-000003
Figure PCTCN2020085514-appb-000003
由表2可知,高效氯氟氰菊酯和甲氨基阿维菌素苯甲酸盐配比范围在20:1-1:20之间,共毒系数都大于120,对小菜蛾防治具有增效作用,尤其在5:1-1:5之间,共毒系数在180以上,增效作用显著。It can be seen from Table 2 that the ratio of lambda-cyhalothrin and emamectin benzoate ranges from 20:1 to 1:20, and the co-toxicity coefficient is greater than 120, which has a synergistic effect on the control of Plutella xylostella The effect, especially between 5:1 and 1:5, the co-toxicity coefficient is above 180, and the synergistic effect is significant.
实施例1:Example 1:
配方:20g高效氯氟氰菊酯、1g甲氨基阿维菌素苯甲酸盐、苯乙烯苯酚聚氧乙烯醚5g、烷基酚聚氧乙烯醚磷酸酯11g、脂肪醇聚氧乙烯醚磷酸酯6g,加水至100g。Formula: 20g lambda-cyhalothrin, 1g emamectin benzoate, styrene phenol polyoxyethylene ether 5g, alkylphenol polyoxyethylene ether phosphate 11g, fatty alcohol polyoxyethylene ether phosphate 6g, add water to 100g.
制备方法:常温(10~35℃)下,称取20g(以有效成分计,下同)高效氯氟氰菊酯原药、1g(以有效成分计,下同)甲氨基阿维菌素苯甲酸盐与5g苯乙烯苯酚聚氧乙烯醚、11g烷基酚聚氧乙烯醚磷酸酯、6g脂肪醇聚氧乙烯醚磷酸酯混合,在转速90转/秒下搅拌0.5h,保持搅拌,加入57g水,继续搅拌0.5h,得到21%高效氯氟氰菊酯·甲维盐纳米水剂。Preparation method: At room temperature (10~35℃), weigh 20g (based on active ingredients, the same below) lambda-cyhalothrin technical and 1g (based on active ingredients, the same below) emamectin benzene The formate is mixed with 5g styrene phenol polyoxyethylene ether, 11g alkylphenol polyoxyethylene ether phosphate, 6g fatty alcohol polyoxyethylene ether phosphate, stir at 90 rpm for 0.5h, keep stirring, add 57g water, continue to stir for 0.5h to obtain 21% lambda-cyhalothrin·emamectin benzoate nano-aqueous agent.
本实施例纳米水剂外观微黄,粘度152mPa·s,平均粒径为15.6纳米。The nano-aqueous agent of this example has a slightly yellow appearance, a viscosity of 152 mPa·s, and an average particle size of 15.6 nanometers.
分别在0℃冷贮7d和54℃热贮14d后制剂均没有发生沉淀现象,仍然稳定。After cold storage at 0°C for 7 days and 54°C heat storage for 14 days, the preparations did not precipitate and remained stable.
本实施例纳米水剂入水后能迅速与水互溶,形成完全透明溶液,稀释稳定性合格。After entering water, the nano-aqueous agent of this embodiment can quickly dissolve with water to form a completely transparent solution, and the dilution stability is qualified.
实施例2:Example 2:
配方:10g高效氯氟氰菊酯、1g甲氨基阿维菌素苯甲酸盐、4g烷基酚甲醛树脂聚氧乙烯醚、2g脂肪醇聚氧乙烯醚、失水山梨醇脂肪酸酯聚氧乙烯醚3g,醇醚琥珀酸单酯磺酸钠4g,加水至100g。Formula: 10g lambda-cyhalothrin, 1g emamectin benzoate, 4g alkylphenol formaldehyde resin polyoxyethylene ether, 2g fatty alcohol polyoxyethylene ether, sorbitan fatty acid ester polyoxygen 3g of vinyl ether, 4g of sodium alcohol ether succinic acid monoester sulfonate, add water to 100g.
制备方法同实施例1,制得11%的高效氯氟氰菊酯·甲维盐纳米水剂。The preparation method is the same as that in Example 1, and 11% lambda-cyhalothrin·emamectin benzoate nano-aqueous agent is prepared.
本实施例纳米水剂外观透明微黄,粘度105mPa·s,平均粒径为15.0纳米。The nano-aqueous agent of this example has a transparent and slightly yellowish appearance, a viscosity of 105 mPa·s, and an average particle size of 15.0 nanometers.
分别在0℃冷贮7d和54℃热贮14d后制剂均没有发生沉淀现象,仍然稳定。After cold storage at 0°C for 7 days and 54°C heat storage for 14 days, the preparations did not precipitate and remained stable.
本实施例纳米水剂入水后能迅速与水互溶,形成完全透明溶液,稀释稳定性合格。After entering water, the nano-aqueous agent of this embodiment can quickly dissolve with water to form a completely transparent solution, and the dilution stability is qualified.
实施例3:Example 3:
配方:5g高效氯氟氰菊酯、1g甲氨基阿维菌素苯甲酸盐、2g烷基酚聚氧乙烯醚磷酸酯、8g苯乙烯基苯酚聚氧乙烯醚,加水至100g。Formula: 5g lambda-cyhalothrin, 1g emamectin benzoate, 2g alkylphenol polyoxyethylene ether phosphate, 8g styrylphenol polyoxyethylene ether, add water to 100g.
制备方法同实施例1,制得6%的高效氯氟氰菊酯·甲维盐纳米水剂。The preparation method is the same as in Example 1, and 6% lambda-cyhalothrin·emamectin benzoate nano-aqueous agent is prepared.
本实施例纳米水剂外观透明微黄,粘度100mPa·s,平均粒径为13.5纳米。The nano-aqueous agent of this example has a transparent and slightly yellow appearance, a viscosity of 100 mPa·s, and an average particle size of 13.5 nanometers.
分别在0℃冷贮7d和54℃热贮14d后制剂均没有发生沉淀现象,仍然稳定。After cold storage at 0°C for 7 days and 54°C heat storage for 14 days, the preparations did not precipitate and remained stable.
本实施例纳米水剂入水后能迅速与水互溶,形成完全透明溶液,稀释稳定性合格。After entering water, the nano-aqueous agent of this embodiment can quickly dissolve with water to form a completely transparent solution, and the dilution stability is qualified.
实施例4:Example 4:
配方:2g高效氯氟氰菊酯、1g甲氨基阿维菌素苯甲酸盐、3g三苯乙烯基苯酚聚氧乙烯醚磷酸酯、4g烷基酚聚氧乙烯醚磷酸酯,加水至100g。Formula: 2g lambda-cyhalothrin, 1g emamectin benzoate, 3g tristyrylphenol polyoxyethylene ether phosphate, 4g alkylphenol polyoxyethylene ether phosphate, add water to 100g.
制备方法同实施例1,制得3%的高效氯氟氰菊酯·甲维盐纳米水剂。The preparation method is the same as that in Example 1, and a 3% lambda-cyhalothrin·emamectin benzoate nano-aqueous agent is prepared.
本实施例纳米水剂外观透明微黄,粘度85.5mPa·s,平均粒径为17.5纳米。The nano-aqueous agent of this example has a transparent and slightly yellowish appearance, a viscosity of 85.5 mPa·s, and an average particle size of 17.5 nanometers.
分别在0℃冷贮7d和54℃热贮14d后制剂均没有发生沉淀现象,仍然稳定。After cold storage at 0°C for 7 days and 54°C heat storage for 14 days, the preparations did not precipitate and remained stable.
本实施例纳米水剂入水后能迅速与水互溶,形成完全透明溶液,稀释稳定性合格。After entering water, the nano-aqueous agent of this embodiment can quickly dissolve with water to form a completely transparent solution, and the dilution stability is qualified.
实施例5:Example 5:
配方:2g高效氯氟氰菊酯、2g甲氨基阿维菌素苯甲酸盐,2g脂肪醇聚氧乙烯醚磷酸酯、3g烷基酚聚氧乙烯醚磷酸酯,加水至100g。Formula: 2g lambda-cyhalothrin, 2g emamectin benzoate, 2g fatty alcohol polyoxyethylene ether phosphate, 3g alkylphenol polyoxyethylene ether phosphate, add water to 100g.
制备方法同实施例1,制得4%的高效氯氟氰菊酯·甲氨基阿维菌素苯甲酸盐纳米水剂。The preparation method is the same as that in Example 1, and a 4% lambda-cyhalothrin·aminoabamectin benzoate nano-water formulation is prepared.
本实施例纳米水剂外观透明微黄,粘度95mPa·s,平均粒径为13纳米。The nano-aqueous agent of this example has a transparent and slightly yellowish appearance, a viscosity of 95 mPa·s, and an average particle size of 13 nanometers.
分别在0℃冷贮7d和54℃热贮14d后制剂均没有发生沉淀现象,仍然稳定。After cold storage at 0°C for 7 days and 54°C heat storage for 14 days, the preparations did not precipitate and remained stable.
本实施例纳米水剂入水后能迅速与水互溶,形成完全透明溶液,稀释稳定性合格。After entering water, the nano-aqueous agent of this embodiment can quickly dissolve with water to form a completely transparent solution, and the dilution stability is qualified.
实施例6:Example 6:
配方:3g高效氯氟氰菊酯、6g甲氨基阿维菌素苯甲酸盐,3g脂肪醇聚氧乙烯醚磷酸酯、4g苯乙烯基苯酚聚氧乙烯醚,加水至100g。Formula: 3g lambda-cyhalothrin, 6g emamectin benzoate, 3g fatty alcohol polyoxyethylene ether phosphate, 4g styrylphenol polyoxyethylene ether, add water to 100g.
制备方法同实施例1,制得9%的高效氯氟氰菊酯·甲维盐纳米水剂。The preparation method is the same as that in Example 1, and 9% lambda-cyhalothrin·emamectin benzoate nano-aqueous agent is prepared.
本实施例纳米水剂外观透明微黄,粘度92mPa·s,平均粒径为15.5纳米。The nano-aqueous agent of this example has a transparent and slightly yellowish appearance, a viscosity of 92 mPa·s, and an average particle size of 15.5 nanometers.
分别在0℃冷贮7d和54℃热贮14d后制剂均没有发生沉淀现象,仍然稳定。After cold storage at 0°C for 7 days and 54°C heat storage for 14 days, the preparations did not precipitate and remained stable.
本实施例纳米水剂入水后能迅速与水互溶,形成完全透明溶液,稀释稳定性合格。After entering water, the nano-aqueous agent of this embodiment can quickly dissolve with water to form a completely transparent solution, and the dilution stability is qualified.
实施例7:Example 7:
配方:2g高效氯氟氰菊酯、10g甲氨基阿维菌素苯甲酸盐,6g苯乙烯基苯酚聚氧乙烯醚、 5g脂肪醇聚氧乙烯醚磷酸酯、加水至100g。Formula: 2g lambda-cyhalothrin, 10g emamectin benzoate, 6g styrylphenol polyoxyethylene ether, 5g fatty alcohol polyoxyethylene ether phosphate, add water to 100g.
制备方法同实施例1,制得12%的高效氯氟氰菊酯·甲维盐纳米水剂。The preparation method is the same as that of Example 1, and 12% lambda-cyhalothrin·emamectin benzoate nano-aqueous agent is prepared.
本实施例纳米水剂外观透明微黄,粘度98mPa·s,平均粒径为14.7纳米。The nano-aqueous agent of this example has a transparent and slightly yellowish appearance, a viscosity of 98 mPa·s, and an average particle size of 14.7 nanometers.
分别在0℃冷贮7d和54℃热贮14d后制剂均没有发生沉淀现象,仍然稳定。After cold storage at 0°C for 7 days and 54°C heat storage for 14 days, the preparations did not precipitate and remained stable.
本实施例纳米水剂入水后能迅速与水互溶,形成完全透明溶液,稀释稳定性合格。After entering water, the nano-aqueous agent of this embodiment can quickly dissolve with water to form a completely transparent solution, and the dilution stability is qualified.
实施例8:Example 8:
配方:1g高效氯氟氰菊酯、10g甲氨基阿维菌素苯甲酸盐,4g醇醚琥珀酸单酯磺酸钠、5g失水山梨醇脂肪酸酯聚氧乙烯醚,3g脂肪醇聚氧乙烯醚,加水至100g。Formula: 1g lambda-cyhalothrin, 10g emamectin benzoate, 4g sodium alcohol ether succinate monoester sulfonate, 5g sorbitan fatty acid ester polyoxyethylene ether, 3g fatty alcohol poly Oxyethylene ether, add water to 100g.
制备方法同实施例1,制得11%的高效氯氟氰菊酯·甲维盐纳米水剂。The preparation method is the same as that in Example 1, and 11% lambda-cyhalothrin·emamectin benzoate nano-aqueous agent is prepared.
本实施例纳米水剂外观透明微黄,粘度105mPa·s,平均粒径为18.6纳米。The nano-aqueous agent of this embodiment has a transparent and slightly yellowish appearance, a viscosity of 105 mPa·s, and an average particle size of 18.6 nanometers.
分别在0℃冷贮7d和54℃热贮14d后制剂均没有发生沉淀现象,仍然稳定。After cold storage at 0°C for 7 days and 54°C heat storage for 14 days, the preparations did not precipitate and remained stable.
本实施例纳米水剂入水后能迅速与水互溶,形成完全透明溶液,稀释稳定性合格。After entering water, the nano-aqueous agent of this embodiment can quickly dissolve with water to form a completely transparent solution, and the dilution stability is qualified.
实施例9:Example 9:
配方:0.5g高效氯氟氰菊酯、10g甲氨基阿维菌素苯甲酸盐,3g苯乙烯基苯酚聚氧乙烯醚、3g三苯乙烯基苯酚聚氧乙烯醚磷酸酯,加水至100g。Formula: 0.5g lambda-cyhalothrin, 10g emamectin benzoate, 3g styrylphenol polyoxyethylene ether, 3g tristyrylphenol polyoxyethylene ether phosphate, add water to 100g.
制备方法同实施例1,制得10.5%的高效氯氟氰菊酯·甲维盐纳米水剂。The preparation method is the same as that in Example 1, and 10.5% lambda-cyhalothrin·emamectin benzoate nano-aqueous agent was prepared.
本实施例纳米水剂外观透明微黄,粘度102mPa·s,平均粒径为15.5纳米。The nano-aqueous agent of this example has a transparent and slightly yellowish appearance, a viscosity of 102 mPa·s, and an average particle size of 15.5 nanometers.
分别在0℃冷贮7d和54℃热贮14d后制剂均没有发生沉淀现象,仍然稳定。After cold storage at 0°C for 7 days and 54°C heat storage for 14 days, the preparations did not precipitate and remained stable.
本实施例纳米水剂入水后能迅速与水互溶,形成完全透明溶液,稀释稳定性合格。After entering water, the nano-aqueous agent of this embodiment can quickly dissolve with water to form a completely transparent solution, and the dilution stability is qualified.
对比例1-对比例4Comparative example 1-Comparative example 4
采用目前配制水剂常用的助剂(润湿剂)配制水剂,具体配方如表3所示。The water preparation is prepared with the commonly used auxiliary (wetting agent) in the preparation of water preparation, and the specific formula is shown in Table 3.
表3.对比例1-对比例4的配方Table 3. Formulations of Comparative Example 1-Comparative Example 4
Figure PCTCN2020085514-appb-000004
Figure PCTCN2020085514-appb-000004
制备方法同实施例1。The preparation method is the same as in Example 1.
按照对比例1和对比例2的配方,在添加助剂的情况下,高效氯氟氰菊酯和甲氨基阿维菌素苯甲酸盐仍然无法完全溶解在水中,不能形成合格的水溶液。According to the formulations of Comparative Example 1 and Comparative Example 2, with the addition of additives, lambda-cyhalothrin and emamectin benzoate still cannot be completely dissolved in water, and a qualified aqueous solution cannot be formed.
按照对比例3和对比例4的配方,在常温(10~35℃)下能够制备获得水溶液,但将水溶液置于低温(0℃以下)下,高效氯氟氰菊酯和甲氨基阿维菌素苯甲酸盐原药会不断析出,而且升温后不可恢复。说明利用非本发明中的表面活性剂或表面活性剂组合物之外的常规水剂使用的表面活性剂无法配制出合格的高效氯氟氰菊酯·甲氨基阿维菌素苯甲酸盐纳米水剂。According to the formulations of Comparative Example 3 and Comparative Example 4, an aqueous solution can be prepared at room temperature (10~35℃), but the aqueous solution is placed at low temperature (below 0℃), lambda-cyhalothrin and emamectin The original benzoic acid salt will continue to precipitate out, and it cannot be recovered after the temperature rises. It shows that the use of surfactants other than the surfactants of the present invention or conventional water agents other than the surfactant composition cannot be used to prepare qualified lambda cyhalothrin·aminoabamectin benzoate nano Water agent.
实施例10:生物活性对比Example 10: Comparison of Biological Activity
田间药效试验一Field efficacy test one
供试药剂:实施例1-实施例9的高效氯氟氰菊酯·甲维盐复配纳米水剂。Test agent: Example 1 to Example 9 Lambda-cyhalothrin·Emmamectin benzoate compound nano-aqueous agent.
防治对象:棉红蜘蛛。Control object: cotton spider mite.
试验方法:采用正常田间使用剂量(有效成分),剂量处理设置三次重复,重复采用随机区组排列,每个重复设置面积30m 2,试验采用背负式喷雾器进行整株棉花喷雾。施药前调查虫口基数,药后3天、7天、14天、30天分别调查残留活虫数,按照以下方法计算防效: Test method: The normal field dosage (active ingredient) was used, the dosage treatment was set for three repetitions, and the random block arrangement was repeated, and the area of each repetition was 30m 2. The experiment used a knapsack sprayer to spray the whole cotton. Investigate the number of insect populations before application, and investigate the number of remaining live insects 3 days, 7 days, 14 days, and 30 days after application, and calculate the control effect according to the following method:
虫口减退率(%)=(施药前虫数-施药后虫数)/施药前虫数×100Insect population reduction rate (%) = (number of insects before application-number of insects after application) / number of insects before application × 100
校正防治效果(%)=(处理区虫口减退率-对照区虫口减退率)/(100-防治前后对照区虫口减退率)×100Corrected control effect (%) = (Reduction rate of insect population in the treatment area-Reduction rate of insect population in the control area) / (100-Recession rate of insect population in the control area before and after control) × 100
处理结果见表4:The treatment results are shown in Table 4:
表4:高效氯氟氰菊酯-甲氨基阿维菌素苯甲酸盐复配对棉红蜘蛛的田间试验结果Table 4: Field test results of Lambda-cyhalothrin-Avermectin benzoate paired with cotton spider mite
Figure PCTCN2020085514-appb-000005
Figure PCTCN2020085514-appb-000005
田间药效结果表明,高效氯氟氰菊酯·甲氨基阿维菌素苯甲酸盐组合物对棉红蜘蛛具有优良 的防治效果,持效期长。The field efficacy results show that the Lambda-cyhalothrin·Avermectin benzoate composition has an excellent control effect on the cotton spider mites and has a long lasting effect.
田间药效试验二Field efficacy test two
供试药剂:实施例1-实施例9的高效氯氟氰菊酯·甲维盐复配纳米水剂。Test agent: Example 1 to Example 9 Lambda-cyhalothrin·Emmamectin benzoate compound nano-aqueous agent.
防除对象:小菜蛾。Control object: Plutella xylostella.
试验方法:采用正常田间使用剂量(有效成分),剂量处理设置三次重复,重复采用随机区组排列,每个重复设置面积50m 2,试验采用背负式喷雾器进行整株棉花喷雾。施药前调查虫口基数,药后3天、7天、14天、30天分别调查残留活虫数,按照以下方法计算防效: Test method: The normal field dosage (active ingredient) was used, the dosage treatment was set for three repetitions, and the random block arrangement was repeated, and the area of each repetition was 50m 2. The experiment used a knapsack sprayer to spray the whole cotton. Investigate the number of insect populations before application, and investigate the number of remaining live insects 3 days, 7 days, 14 days, and 30 days after application, and calculate the control effect according to the following method:
虫口减退率(%)=(施药前虫数-施药后虫数)/施药前虫数×100Insect population reduction rate (%) = (number of insects before application-number of insects after application) / number of insects before application × 100
校正防治效果(%)=(处理区虫口减退率-对照区虫口减退率)/(100-防治前后对照区虫口减退率)×100Corrected control effect (%) = (Reduction rate of insect population in the treatment area-Reduction rate of insect population in the control area) / (100-Recession rate of insect population in the control area before and after control) × 100
表5:高效氯氟氰菊酯-甲氨基阿维菌素苯甲酸盐复配对小菜蛾的田间试验结果Table 5: Field test results of Lambda-cyhalothrin-Avermectin benzoate paired with Plutella xylostella
Figure PCTCN2020085514-appb-000006
Figure PCTCN2020085514-appb-000006
田间药效结果表明,高效氯氟氰菊酯·甲氨基阿维菌素苯甲酸盐组合物对小菜蛾具有优良的防治效果,持效期长。Field efficacy results show that the Lambda-cyhalothrin·Avermectin benzoate composition has an excellent control effect on Plutella xylostella and has a long lasting effect.

Claims (9)

  1. 一种含高效氯氟氰菊酯和甲氨基阿维菌素苯甲酸盐的复合杀虫杀螨纳米水剂,其特征在于所述的纳米水剂以高效氯氟氰菊酯和甲氨基阿维菌素苯甲酸盐为活性成分,与表面活性剂、水配制成的,所述纳米水剂中,高效氯氟氰菊酯和甲氨基阿维菌素苯甲酸盐的重量百分含量为3~50%,表面活性剂的重量百分含量为5~20%,余量为水。A composite insecticidal and acaricidal nano-aqueous agent containing lambda-cyhalothrin and emamectin benzoate, characterized in that the nano-aqueous agent is made of lambda-cyhalothrin and methylamino-abamectin benzoate. Vermectin benzoate is the active ingredient and is formulated with surfactants and water. In the nano-aqueous agent, the weight percentages of lambda-cyhalothrin and emamectin benzoate It is 3-50%, the weight percentage of the surfactant is 5-20%, and the balance is water.
  2. 根据权利要求1所述的纳米水剂,其特征在于所述的纳米水剂中,高效氯氟氰菊酯和甲氨基阿维菌素苯甲酸盐的重量百分含量为3~21%。The nano-aqueous agent according to claim 1, wherein the weight percentage of lambda-cyhalothrin and emamectin benzoate in the nano-aqueous agent is 3-21%.
  3. 根据权利要求1所述的纳米水剂,其特征在于所述的高效氯氟氰菊酯和甲氨基阿维菌素苯甲酸盐的重量比为20:1~1:20。The nano-aqueous agent according to claim 1, wherein the weight ratio of the lambda-cyhalothrin and emamectin benzoate is 20:1 to 1:20.
  4. 根据权利要求1所述的纳米水剂,其特征在于所述的高效氯氟氰菊酯和甲氨基阿维菌素苯甲酸盐的重量比为5:1-1:5。The nano-aqueous agent according to claim 1, wherein the weight ratio of the lambda-cyhalothrin and emamectin benzoate is 5:1 to 1:5.
  5. 根据权利要求1所述的纳米水剂,其特征在于所述的表面活性剂选自脂肪醇聚氧乙烯醚、烷基酚甲醛树脂聚氧乙烯醚、苯乙烯基苯酚聚氧乙烯醚、脂肪醇聚氧乙烯醚磷酸酯、三苯乙烯基苯酚聚氧乙烯醚磷酸酯、烷基酚聚氧乙烯醚磷酸酯、醇醚琥珀酸单酯磺酸钠、失水山梨醇脂肪酸酯聚氧乙烯醚中的一种或者多种组合。The nano-aqueous agent according to claim 1, wherein the surfactant is selected from fatty alcohol polyoxyethylene ether, alkylphenol formaldehyde resin polyoxyethylene ether, styrylphenol polyoxyethylene ether, fatty alcohol Polyoxyethylene ether phosphate, tristyryl phenol polyoxyethylene ether phosphate, alkylphenol polyoxyethylene ether phosphate, alcohol ether succinic acid monoester sodium sulfonate, sorbitan fatty acid ester polyoxyethylene ether One or more combinations of.
  6. 权利要求1所述的纳米水剂的制备方法,其特征在于所述制备方法包括以下步骤:The preparation method of nano-aqueous agent according to claim 1, characterized in that the preparation method comprises the following steps:
    步骤(1)、在常温下,将高效氯氟氰菊酯原药、甲氨基阿维菌素苯甲酸盐原药与表面活性剂混合,搅拌,使高效氯氟氰菊酯和甲氨基阿维菌素苯甲酸盐均匀分散在表面活性剂中;Step (1), at room temperature, the lambda-cyhalothrin technical medicine, emamectin benzoate technical medicine and the surfactant are mixed, and stirred to make lambda-cyhalothrin and methylamino amethyrin Vermectin benzoate is evenly dispersed in the surfactant;
    步骤(2)、在搅拌状态下加入水,搅拌均匀,形成含有高效氯氟氰菊酯和甲氨基阿维菌素苯甲酸盐的表面活性剂胶束溶液,即为透明的高效氯氟氰菊酯和甲氨基阿维菌素苯甲酸盐纳米水剂。Step (2). Add water under stirring and stir evenly to form a surfactant micellar solution containing lambda-cyhalothrin and emamectin benzoate, which is a transparent lambda-chlorofluorocyanate Pyrethrin and emamectin benzoate nano-aqueous agent.
  7. 根据权利要求6所述的纳米水剂的制备方法,其特征在于步骤(1)和步骤(2)中,所述搅拌速度为60~100转/秒。The preparation method of nano-aqueous agent according to claim 6, characterized in that in step (1) and step (2), the stirring speed is 60-100 revolutions per second.
  8. 根据权利要求1所述的纳米水剂在防治果树、棉花、蔬菜上的害虫、害螨的用途。The use of the nano-aqueous agent according to claim 1 to control pests and mites on fruit trees, cotton and vegetables.
  9. 根据权利要求8所述的用途,其特征在于所述的害虫为小菜蛾,所述的害螨为棉红蜘蛛。The use according to claim 8, characterized in that the pest is Plutella xylostella, and the pest mite is cotton spider mite.
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