CN110973154A - Composite insecticidal and acaricidal nano water agent containing fenpropathrin and emamectin benzoate and application thereof - Google Patents
Composite insecticidal and acaricidal nano water agent containing fenpropathrin and emamectin benzoate and application thereof Download PDFInfo
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Abstract
The invention discloses a composite insecticidal and acaricidal nano-water agent containing fenpropathrin and emamectin benzoate, wherein the insecticidal composition takes the fenpropathrin and the emamectin benzoate as insecticidal and acaricidal active ingredients, the weight percentage content of the fenpropathrin and the emamectin benzoate is 3-25%, the weight percentage content of a pesticide auxiliary agent is 5-20%, and the balance is water. The weight ratio of the fenpropathrin to the emamectin benzoate is 20:1-1: 20. The invention utilizes the nano micelle formed by the surfactant to bear the fenpropathrin and the emamectin benzoate which are difficult to dissolve in water, and the effective components exist in the nano water agent as nano particles, thereby being beneficial to the attachment, the distribution and the permeation of the nano water agent on a target and being more resistant to rain wash. The two effective components can generate a synergistic interaction effect, can prevent and control lepidoptera pests and mite pests on crops, and has the advantages of high insecticidal speed, long lasting period and obviously higher prevention and control effect than that of a single agent.
Description
Technical Field
The invention belongs to the field of pesticides, and relates to a composite insecticidal and acaricidal nano-water agent containing fenpropathrin and emamectin benzoate and application thereof.
Background
Fenpropathrin (Fenpropathrin), chemical name: 2-cyano-3-phenoxybenzyl-2, 2,3, 3-tetramethylcyclopropanecarboxylate. High efficiency, broad spectrum pyrethroid, contact poisoning and repelling effect, and stomach poisoning effect. Besides the characteristics of general pyrethrin, the insecticidal composition has good effect on various crop spider mites, so that the insecticidal composition has the advantage of killing insects and mites. It is effective on Lepidoptera larva, and diptera or Hemiptera pest. Can be used for preventing and treating pests on cotton, fruit trees, vegetables, tea leaves and flowers.
Emamectin Benzoate, abbreviated as Emamectin Benzoate, has the molecular formula: c56H81NO15. Chemical name: 4 '-epi-methylamino-4' -deoxyabamectin B1 benzoate. The emamectin benzoate is a novel high-efficiency semi-synthetic antibiotic pesticide synthesized from a fermentation product abamectin B1, and has the characteristics of super-high efficiency, low toxicity (the preparation is nearly nontoxic), low residue, no public nuisance and other biological pesticides. Is widely used for preventing and controlling various pests on crops such as vegetables, fruit trees, cotton and the like.
Pesticide varieties containing a single component often have defects in pesticide pest control: the pesticide resistance is easy to generate after continuous use, the insecticidal spectrum is narrow, the comprehensive protection can not be provided for crops, the pesticide cost of farmers is high, and the like. The combination and blending of two or more active ingredients with synergistic effect can improve the control effect, reduce the dosage of the active ingredients, save the cost, slow down the resistance of pests and mites, expand the control spectrum, play a role in controlling multiple pests and reduce the use cost of farmers.
Because fenpropathrin is poorly soluble in water, the solubility in water at 20 ℃ is only 0.34ppm, emamectin benzoate is slightly soluble in water. At present, the conventional formulations of fenpropathrin and emamectin benzoate are mainly missible oil containing a large amount of organic solvents, so that potential safety hazards exist in production, and serious harm is caused to the environment in field use. The use of organic solvent is reduced, and the development of aqueous preparation formulation is a necessary way for the development of fenpropathrin and emamectin benzoate.
Disclosure of Invention
The invention aims to provide a composite insecticidal and acaricidal nano-water agent containing fenpropathrin and emamectin benzoate, wherein the compounding of the fenpropathrin and emamectin benzoate in the nano-water agent has obvious synergistic effect; in addition, under the condition of not using an organic solvent for assisting dissolution, a certain specific surfactant is creatively adopted, and through a surfactant micelle solubilization technology, the nano-scale micelle formed by the surfactant is used for bearing the fenpropathrin and the emamectin benzoate which are difficult to dissolve in water, so that the effective components exist in the nano-water agent as nano-scale particles, the nano-water agent is more convenient to attach, spread and permeate on a target and is more resistant to rain washing, and the nano-water agent does not contain an organic solvent, and is safe and environment-friendly.
The purpose of the invention is realized by the following technical scheme:
a composite insecticidal and acaricidal nano-water agent containing fenpropathrin and emamectin benzoate is prepared by taking fenpropathrin and emamectin benzoate as active ingredients, a surfactant and water; the weight ratio of the fenpropathrin to the emamectin benzoate is 20:1-1:20, the weight percentage content of the fenpropathrin to the emamectin benzoate is 3-25%, the weight percentage content of the pesticide auxiliary agent is 5-20%, and the balance is water.
The nano water agent is prepared by adopting a surfactant micelle solubilization technology.
Preferably, the weight ratio of the fenpropathrin to the emamectin benzoate is 1: 5-5: 1.
In the nano water agent, the weight percentage content of the fenpropathrin and the emamectin benzoate is preferably 3-12%.
The surfactant is selected from fatty alcohol-polyoxyethylene ether, alkylphenol formaldehyde resin polyoxyethylene ether, styryl phenol polyoxyethylene ether, fatty alcohol-polyoxyethylene ether sodium sulfate, alcohol ether succinic acid monoester sodium sulfonate, alkylphenol polyoxyethylene ether phosphate, fatty acid methyl ester sodium sulfonate and the like, and the surfactants can be used singly or in combination.
The invention also aims to provide a preparation method of the composite insecticidal and acaricidal nano water agent containing fenpropathrin and emamectin benzoate, which comprises the following steps:
step (1), mixing and stirring fenpropathrin and emamectin benzoate raw materials and a surfactant at normal temperature (10-35 ℃) to uniformly disperse the fenpropathrin and the emamectin benzoate in the surfactant;
and (2) adding water under the stirring state, and uniformly stirring to form a surfactant micelle solution containing fenpropathrin and emamectin benzoate, namely the transparent composite insecticidal and acaricidal nano water agent containing fenpropathrin and emamectin benzoate. The fenpropathrin and emamectin benzoate nano water aqua is transparent in appearance, and the average particle size of the surfactant micelle is in a nano level; after entering water, the water-soluble polymer can be quickly dissolved with water to form a completely transparent solution, and the dilution stability is qualified; the nano water aqua of the invention is still stable after being stored for 7 days at 0 ℃ and stored for 14 days at 54 ℃ respectively, fenpropathrin can not be separated out, the performance is stable, and the nano water aqua is convenient to store.
In the step (1), the stirring speed is 60-100 revolutions per second, and the stirring time is generally 0.5h, so that the fenpropathrin and the emamectin benzoate are uniformly dispersed in the surfactant.
In the step (2), the stirring speed is 60-100 r/s, and the stirring is continued for 0.5-1 h after the water is added.
The invention also aims to provide the application of the nano water aqua in preventing and treating pests and mites on fruit trees, cotton and vegetables. The pest is cotton bollworm, and the pest mite is cotton red spider. In the using process, the dosage can be reduced, the generation of drug resistance of pests and mites can be delayed, the control effect can be improved, the use is better than that of a single agent, the time and the labor are saved, the cost is saved, the pollution to the environment is reduced, and the burden of farmers is lightened.
Compared with the prior art, the invention has the beneficial effects that:
(1) the compound has obvious synergistic effect, and improves the control effect on pest mites compared with the single dose which is used independently;
(2) has quick and long-acting effects;
(3) the two effective components are compounded, so that the using amount of the pesticide is reduced, and the production and use cost and the pollution to the environment are reduced;
(4) the resistance of the pest mites to pesticides is delayed, and the effect is obviously higher than that of the pest mites used in a single dose.
Drawings
Fig. 1 shows 10.5% fenpropathrin emamectin benzoate nano-water aqua in example 9.
FIG. 2 is a 10.5% unqualified aqueous solution of fenpropathrin-emamectin benzoate of comparative example 2.
Detailed Description
The invention is further illustrated but is not in any way limited by the following examples.
Indoor virulence determination
1. Carrying out toxicity determination on the cotton red spider by adopting a dipping slide method for fenpropathrin, emamectin benzoate and compound samples thereof, repeating for 3 times each treatment, treating for 30 heads each concentration, and using LC50Values co-toxicity coefficients (CTC values) were calculated according to the grandsinope method:
single dose of LC50 as standard medicine/single dose of LC 50X 100
Theoretical virulence index (TTI) ═ A virulence index of single agent, x proportion of single agent in mixed agent + B virulence index, x proportion of single agent in mixed agent
Measured virulence index (ATI) ═ standard single dose LC50 value/LC 50 value of the mix × 100
Co-toxicity coefficient (CTC) measured toxicity index (ATI)/Theoretical Toxicity Index (TTI) x 100
Grading co-toxicity coefficients: the mixture has synergistic effect when CTC is greater than 120, is antagonistic when CTC is less than 80, and has additive effect between 80 and 120.
The results are shown in Table 1.
TABLE 1 indoor toxicity assay for cotton red spider using composite of fenpropathrin and emamectin benzoate
As can be seen from Table 1, the mixture ratio of the fenpropathrin to the emamectin benzoate ranges from 20:1 to 1:20, the co-toxicity coefficients are all larger than 120, the synergistic effect on the prevention and treatment of the cotton red spider is achieved, particularly the co-toxicity coefficient ranges from 5:1 to 1:5, the co-toxicity coefficient is over 160, and the synergistic effect is obvious.
2. Adopting a feed mixed toxicity method, selecting cotton bollworms as target pests, repeating the treatment for three times, and calculating a toxicity regression equation and lethal medium concentration LC of each medicament on the cotton bollworms by using a probability value method50By LC50The results of the co-measure coefficient calculation according to the Sun cloud Peel method are shown in Table 2.
TABLE 2 toxicity assay of composite pairs of fenpropathrin and emamectin benzoate for Heliothis armigera
As can be seen from Table 2, the mixture ratio of the fenpropathrin to the emamectin benzoate ranges from 20:1 to 1:20, the co-toxicity coefficients are all larger than 120, the synergistic effect on the control of the cotton bollworm is achieved, particularly the co-toxicity coefficient ranges from 5:1 to 1:5, the co-toxicity coefficient is more than 170, and the synergistic effect is obvious.
Example 1:
the formula is as follows: 20g of fenpropathrin, 1g of emamectin benzoate, 10g of fatty alcohol-polyoxyethylene ether, 5g of alkylphenol formaldehyde resin polyoxyethylene and water until the weight is 100 g.
The preparation method comprises the following steps: weighing 20g (calculated by effective components, the same below) of fenpropathrin original drug, 1g of emamectin benzoate, 10g of fatty alcohol-polyoxyethylene ether and 5g of alkylphenol formaldehyde resin polyoxyethylene, mixing, stirring for 0.5h at the rotating speed of 85 revolutions per second, keeping stirring, adding 64g of water, and continuously stirring for 1h to obtain 21% of fenpropathrin-emamectin benzoate nano-water agent.
The nano water agent of the embodiment has transparent and yellowish appearance, viscosity of 180 mPa.s and average particle size of 12.0 nm.
The nano water agent of the embodiment has no precipitation phenomenon after being stored at 0 ℃ for 7 days and at 54 ℃ for 14 days respectively, and is still stable.
The nano water agent can be quickly dissolved with water after entering water to form a completely transparent solution, and the dilution stability is qualified.
Example 2:
the formula is as follows: 10g of fenpropathrin, 1g of emamectin benzoate, 3g of styryl phenol polyoxyethylene ether, 3g of fatty alcohol-polyoxyethylene ether, 2g of alkylphenol formaldehyde resin polyoxyethylene ether and water until the weight is 100 g.
The preparation method is the same as that of the example 1, and the fenpropathrin-emamectin benzoate nano-water aqua with the concentration of 11 percent is prepared.
The nano water agent of the embodiment has transparent and yellowish appearance, viscosity of 195 mPas and average particle size of 13.6 nm.
The nano water agent of the embodiment has no precipitation phenomenon after being stored at 0 ℃ for 7 days and at 54 ℃ for 14 days respectively, and is still stable.
The nano water agent can be quickly dissolved with water after entering water to form a completely transparent solution, and the dilution stability is qualified.
Example 3:
the formula is as follows: 5g of fenpropathrin, 1g of emamectin benzoate, 1g of alkylphenol formaldehyde resin polyoxyethylene ether, 3g of fatty alcohol-polyoxyethylene ether sodium sulfate and water until the weight is 100 g.
The preparation method is the same as that of the example 1, and 6 percent of fenpropathrin-emamectin benzoate nano-water aqua is prepared.
The nano water agent of the embodiment has transparent and yellowish appearance, viscosity of 185mPa & s and average particle size of 18.5 nm.
The nano water agent of the embodiment has no precipitation phenomenon after being stored at 0 ℃ for 7 days and at 54 ℃ for 14 days respectively, and is still stable.
The nano water agent can be quickly dissolved with water after entering water to form a completely transparent solution, and the dilution stability is qualified.
Example 4:
the formula is as follows: 2g of fenpropathrin, 1g of emamectin benzoate, 4g of sodium alcohol ether succinate monoester sulfonate, 3g of alkylphenol polyoxyethylene phosphate and water until the weight is 100 g.
The preparation method is the same as that of the example 1, and the 3 percent fenpropathrin-emamectin benzoate nano-water aqua is prepared.
The nano water agent of the embodiment has transparent and yellowish appearance, viscosity of 200 mPas and average particle size of 18.0 nm.
The nano water agent of the embodiment has no precipitation phenomenon after being stored at 0 ℃ for 7 days and at 54 ℃ for 14 days respectively, and is still stable.
The nano water agent can be quickly dissolved with water after entering water to form a completely transparent solution, and the dilution stability is qualified.
Example 5:
the formula is as follows: 2g of fenpropathrin, 2g of emamectin benzoate, 2g of alkylphenol formaldehyde resin polyoxyethylene ether, 3g of alkylphenol polyoxyethylene ether phosphate and water until the weight is 100 g.
The preparation method is the same as that of the example 1 to prepare the 4 percent fenpropathrin-emamectin benzoate nano water agent.
The nano water agent of the embodiment has transparent and yellowish appearance, viscosity of 202 mPas and average particle size of 17.8 nm.
The nano water agent of the embodiment has no precipitation phenomenon after being stored at 0 ℃ for 7 days and at 54 ℃ for 14 days respectively, and is still stable.
The nano water agent can be quickly dissolved with water after entering water to form a completely transparent solution, and the dilution stability is qualified.
Example 6:
the formula is as follows: 3g of fenpropathrin, 6g of emamectin benzoate, 2g of sodium alcohol ether succinate monoester sulfonate, 1g of styryl phenol polyoxyethylene ether and water until the weight is 100 g.
The preparation method is the same as that of the example 1, and 9 percent of fenpropathrin-emamectin benzoate nano-water aqua is prepared.
The nano water agent of the embodiment has transparent and yellowish appearance, viscosity of 157 mPas and average particle size of 13.8 nm.
The nano water agent of the embodiment has no precipitation phenomenon after being stored at 0 ℃ for 7 days and at 54 ℃ for 14 days respectively, and is still stable.
The nano water agent can be quickly dissolved with water after entering water to form a completely transparent solution, and the dilution stability is qualified.
Example 7:
weighing 2g of fenpropathrin, 10g of emamectin benzoate, 5g of styryl phenol polyoxyethylene ether, 2g of alkylphenol polyoxyethylene ether phosphate and water to 100 g.
The preparation method is the same as that of the example 1, and the 12 percent fenpropathrin-emamectin benzoate nano water agent is prepared.
The nano water agent of the embodiment has transparent and yellowish appearance, viscosity of 180 mPa.s and average particle size of 15.5 nm.
The nano water agent of the embodiment has no precipitation phenomenon after being stored at 0 ℃ for 7 days and at 54 ℃ for 14 days respectively, and is still stable.
The nano water agent can be quickly dissolved with water after entering water to form a completely transparent solution, and the dilution stability is qualified.
Example 8:
weighing 1g of fenpropathrin, 10g of emamectin benzoate, 4g of fatty alcohol-polyoxyethylene ether sodium sulfate, 3g of fatty acid methyl ester sodium sulfonate and 2g of alkylphenol polyoxyethylene ether phosphate, and adding water to 100 g.
The preparation method is the same as that of the example 1, and the fenpropathrin-emamectin benzoate nano-water aqua with the concentration of 11 percent is prepared.
The nano water agent of the embodiment has transparent and yellowish appearance, viscosity of 170 mPa.s and average particle size of 19.6 nm.
The nano water agent of the embodiment has no precipitation phenomenon after being stored at 0 ℃ for 7 days and at 54 ℃ for 14 days respectively, and is still stable.
The nano water agent can be quickly dissolved with water after entering water to form a completely transparent solution, and the dilution stability is qualified.
Example 9:
weighing 0.5g of fenpropathrin, 10g of emamectin benzoate, 4g of styrylphenol polyoxyethylene ether and 100g of alkylphenol formaldehyde resin polyoxyethylene, and adding water.
The preparation method is the same as the example 1, and the 10.5 percent fenpropathrin-emamectin benzoate nano water agent is prepared.
The nano water agent of the embodiment has transparent and yellowish appearance (see figure 1), viscosity of 185mPa & s and average particle size of 20.7 nm.
The nano water agent of the embodiment has no precipitation phenomenon after being stored at 0 ℃ for 7 days and at 54 ℃ for 14 days respectively, and is still stable.
The nano water agent can be quickly dissolved with water after entering water to form a completely transparent solution, and the dilution stability is qualified.
Comparative examples 1 to 4
The water aqua is prepared by adopting the commonly used auxiliary agent (wetting agent) for preparing the water aqua at present, and the specific formula is shown in table 3.
TABLE 3 formulations of comparative examples 1 to 4
According to the formulations of comparative example 1 and comparative example 2, according to the preparation method of example 1, with the addition of the adjuvant, fenpropathrin and emamectin benzoate still do not dissolve completely in water and do not form a passing aqueous solution (fig. 2 is a failing aqueous solution obtained according to the formulation of comparative example 2).
According to the formulas of the comparative example 3 and the comparative example 4 and the preparation method of the example 1, the aqueous solution can be prepared at normal temperature (10-35 ℃), but when the aqueous solution is placed at low temperature (below 0 ℃), raw fenpropathrin and emamectin benzoate are continuously separated out and cannot be recovered after being heated.
It is demonstrated that the surfactant used by the conventional water aqua other than the surfactant of the invention can not be used for preparing qualified fenpropathrin-emamectin benzoate nano water aqua.
Example 10: comparison of biological Activity
Test of field drug effect
Reagent to be tested: example 1-the fenpropathrin-emamectin benzoate compound nano-water aqua of example 9.
The control object is: spider mites of the Gossypium hirsutum.
The test method comprises the following steps: adopting normal field dosage (effective component), setting three times of repetition of dosage treatment, repeatedly adopting random block arrangement, and setting area of each repetition to be 30m2The whole cotton is sprayed by a knapsack sprayer. Investigating population base before application, investigating residual live insect number 3 days, 7 days, 14 days and 30 days after application, and calculating the control effect according to the following method:
percent reduction rate (%) of population (number of insects before application-number of insects after application)/number of insects before application × 100
Correction control effect (%) - (treatment area oral cavity decline rate-control area oral cavity decline rate)/(100-control area oral cavity decline rate before and after control) × 100
The results of the treatment are shown in Table 4.
Table 4: results of field test of fenpropathrin-emamectin benzoate nano water aqua on cotton red spider
The field pesticide effect result shows that the fenpropathrin-emamectin benzoate composition has excellent control effect on the cotton red spider and long lasting period.
Table 5: results of field test of fenpropathrin-emamectin benzoate nano water aqua on cotton bollworm
The field pesticide effect result shows that the fenpropathrin-emamectin benzoate composition has excellent control effect on cotton bollworm and long lasting period.
Claims (8)
1. A composite insecticidal and acaricidal nano-water agent containing fenpropathrin and emamectin benzoate is characterized in that the nano-water agent is prepared by taking fenpropathrin and emamectin benzoate as active ingredients, a surfactant and water; the weight ratio of the fenpropathrin to the emamectin benzoate is 20:1-1:20, the weight percentage content of the fenpropathrin to the emamectin benzoate is 3-25%, the weight percentage content of the pesticide auxiliary agent is 5-20%, and the balance is water.
2. The nano-water agent of claim 1, wherein the nano-water agent is prepared by a surfactant micelle solubilization technique.
3. The nano water aqua according to claim 1, wherein the weight ratio of fenpropathrin to emamectin benzoate is 5:1-1: 5.
4. The nano-water agent as claimed in claim 1, wherein the surfactant is selected from one or more of fatty alcohol-polyoxyethylene ether, alkylphenol formaldehyde resin polyoxyethylene ether, styrylphenol polyoxyethylene ether, sodium fatty alcohol-polyoxyethylene ether sulfate, sodium alcohol ether succinate monoester sulfonate, alkylphenol polyoxyethylene ether phosphate, and sodium fatty acid methyl ester sulfonate.
5. The method for preparing a nano-water agent according to claim 1, which comprises:
mixing and stirring fenpropathrin and emamectin benzoate raw materials and a surfactant at normal temperature to uniformly disperse the fenpropathrin and the emamectin benzoate in the surfactant;
and (2) adding water under the stirring state, and uniformly stirring to obtain the composite insecticidal and acaricidal nano water agent containing fenpropathrin and emamectin benzoate.
6. The method for preparing the nano water aqua according to claim 5 is characterized in that in the step (1), the stirring speed is 60-100 revolutions per second; in the step (2), the stirring speed is 60-100 rpm/s.
7. The use of the nano water aqua according to claim 1 for controlling pests and mites of fruit trees, cotton and vegetables.
8. The use according to claim 1, characterized in that the pests are cotton bollworms and the mites are spider mites.
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| PCT/CN2020/085762 WO2021093270A1 (en) | 2019-11-13 | 2020-04-21 | Compound insecticidal and acaricidal nano aqueous formulation containing fenpropathrin and emamectin benzoate, and use thereof |
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| CN110999902A (en) * | 2019-11-13 | 2020-04-14 | 南京华洲药业有限公司 | Nanometer water agent containing prochloraz and processing method thereof |
| CN110973154A (en) * | 2019-11-13 | 2020-04-10 | 南京华洲药业有限公司 | Composite insecticidal and acaricidal nano water agent containing fenpropathrin and emamectin benzoate and application thereof |
| CN110973125A (en) * | 2019-11-13 | 2020-04-10 | 南京华洲药业有限公司 | Nanometer water agent containing acetochlor and processing method thereof |
-
2019
- 2019-11-13 CN CN201911109335.6A patent/CN110973154A/en not_active Withdrawn
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2020
- 2020-04-21 WO PCT/CN2020/085762 patent/WO2021093270A1/en active Application Filing
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| WO2021093266A1 (en) * | 2019-11-11 | 2021-05-20 | 南京华洲药业有限公司 | Compound insecticidal and acaricidal nano aqueous formulation containing lambda-cyhalothrin and emamectin benzoate, and use thereof |
| WO2021093267A1 (en) * | 2019-11-12 | 2021-05-20 | 南京华洲药业有限公司 | Composite insecticidal and acaricidal nano-aqueous agent containing fenpropathrin and chlorpyrifos, and preparation method therefor and use thereof |
| WO2021093268A1 (en) * | 2019-11-12 | 2021-05-20 | 南京华洲药业有限公司 | High-efficiency cyhalothrin nano aqueous solution, preparation method therefor and application thereof |
| WO2021093270A1 (en) * | 2019-11-13 | 2021-05-20 | 南京华洲药业有限公司 | Compound insecticidal and acaricidal nano aqueous formulation containing fenpropathrin and emamectin benzoate, and use thereof |
| WO2021093269A1 (en) * | 2019-11-13 | 2021-05-20 | 南京华洲药业有限公司 | Nano aqueous agent comprising prochloraz and processing method therefor |
| CN116253626A (en) * | 2023-03-10 | 2023-06-13 | 中国农业科学院农业环境与可持续发展研究所 | Alcohol ether compound and application thereof in water-based nano pesticide preparation |
| CN116253626B (en) * | 2023-03-10 | 2023-09-01 | 中国农业科学院农业环境与可持续发展研究所 | Alcohol ether compound and application thereof in water-based nano pesticide preparation |
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Application publication date: 20200410 |