CN114097797B - Insecticidal composition, insecticide with multiple functions, and preparation method and application thereof - Google Patents

Insecticidal composition, insecticide with multiple functions, and preparation method and application thereof Download PDF

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CN114097797B
CN114097797B CN202111441647.4A CN202111441647A CN114097797B CN 114097797 B CN114097797 B CN 114097797B CN 202111441647 A CN202111441647 A CN 202111441647A CN 114097797 B CN114097797 B CN 114097797B
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ferulic
aldehyde
chlorantraniliprole
lufenuron
insecticidal
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CN114097797A (en
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陈文杰
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Liyang Zhongnan Chemical Industry Co ltd
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Liyang Zhongnan Chemical Industry Co ltd
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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
    • A01N43/00Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/48Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with two nitrogen atoms as the only ring hetero atoms
    • A01N43/561,2-Diazoles; Hydrogenated 1,2-diazoles
    • 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
    • A01N35/00Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having two bonds to hetero atoms with at the most one bond to halogen, e.g. aldehyde radical
    • A01N35/02Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having two bonds to hetero atoms with at the most one bond to halogen, e.g. aldehyde radical containing aliphatically bound aldehyde or keto groups, or thio analogues thereof; Derivatives thereof, e.g. acetals
    • 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
    • A01N35/00Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having two bonds to hetero atoms with at the most one bond to halogen, e.g. aldehyde radical
    • A01N35/08Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having two bonds to hetero atoms with at the most one bond to halogen, e.g. aldehyde radical at least one of the bonds to hetero atoms is to nitrogen
    • A01N35/10Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having two bonds to hetero atoms with at the most one bond to halogen, e.g. aldehyde radical at least one of the bonds to hetero atoms is to nitrogen containing a carbon-to-nitrogen double bond
    • 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
    • A01N47/00Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid
    • A01N47/08Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid the carbon atom having one or more single bonds to nitrogen atoms
    • A01N47/28Ureas or thioureas containing the groups >N—CO—N< or >N—CS—N<
    • A01N47/34Ureas or thioureas containing the groups >N—CO—N< or >N—CS—N< containing the groups, e.g. biuret; Thio analogues thereof; Urea-aldehyde condensation products

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  • Engineering & Computer Science (AREA)
  • Agronomy & Crop Science (AREA)
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Abstract

The application relates to the technical field of pesticides, in particular to an insecticidal composition, a pesticide with multiple functions, a preparation method and application thereof. The insecticidal composition provided by the application comprises the following components in parts by weight: 16-21.5 parts of insecticidal active ingredients, 3.5-4.2 parts of sodium alkyl sulfonate, 3.0-4.0 parts of polyarylphenol polyether phosphate, 2.8-3.1 parts of antifreezing agent, 0.5-0.7 parts of defoamer, 0.1-0.2 parts of thickener and 0.1-0.15 parts of preservative, wherein the insecticidal active ingredients comprise chlorantraniliprole and lufenuron in a weight ratio of 5.2-6.6:11.0-12.7. The insecticidal composition and the insecticide with multiple functions adopt chlorantraniliprole and lufenuron as the insecticidal active ingredients, and the chlorantraniliprole and lufenuron can be synergistic and double-insecticidal, so that the control effect is improved.

Description

Insecticidal composition, insecticide with multiple functions, and preparation method and application thereof
Technical Field
The application relates to the technical field of pesticides, in particular to an insecticidal composition, a pesticide with multiple functions, a preparation method and application thereof.
Background
In the modern agricultural process, pesticides play a very important role, and the use of pesticides has become very effective measures for increasing yield, protecting yield and improving efficiency in agricultural production. The agricultural pesticide is the most widely used one in pesticides, and can prevent and treat diseases and insect pests and improve the yield of crops. The agricultural pesticides used at present have strong pertinence, and different pesticides or multiple pesticides are selected for compounding for different pests.
Spodoptera frugiperda belongs to spodoptera of lepidopteridae, is a worldwide serious pest, is native to tropical subtropical areas of america, and is probably migrated into China in 2019 and is fast in diffusion. The use of pesticides to rapidly compact populations and mitigate hazards is currently the primary method of controlling spodoptera frugiperda. However, spodoptera frugiperda has a high resistance to organophosphorus, pyrethroid and carbamate pesticides in america, which brings great trouble to control of spodoptera frugiperda. In addition, the action of the grass greedy night is hidden, and the instability is brought to the control effect of the pesticide.
At present, emamectin benzoate, acetamiprid, cyhalothrin and the like are mainly used for preventing and controlling spodoptera frugiperda in China, but the inventor finds that the prevention effect of the insecticide on spodoptera frugiperda is gradually reduced along with the large-area use of the emamectin benzoate, acetamiprid, cyhalothrin and the like in the actual use process. Therefore, aiming at the characteristics of hidden activity and strong drug resistance of spodoptera frugiperda, development of an insecticide with higher control effect is needed.
Disclosure of Invention
In order to improve the insecticidal effect, the application provides an insecticidal composition, an insecticide with multiple functions, and a preparation method and application thereof.
In a first aspect, the present application provides an insecticidal composition according to the following technical scheme:
an insecticidal composition comprises the following components in parts by weight: 16-21.5 parts of insecticidal active ingredients, 3.5-4.2 parts of sodium alkyl sulfonate, 3.0-4.0 parts of polyarylphenol polyether phosphate, 2.8-3.1 parts of antifreezing agent, 0.5-0.7 parts of defoamer, 0.1-0.2 parts of thickener and 0.1-0.15 parts of preservative, wherein the insecticidal active ingredients comprise chlorantraniliprole and lufenuron in a weight ratio of 5.2-6.6:11.0-12.7.
By adopting the technical scheme, the insecticidal effective components contain chlorantraniliprole and lufenuron, so that the strong stomach toxicity of the chlorantraniliprole and the strong contact insecticidal effect of lufenuron can be utilized to form multiple insecticidal effects on pests such as spodoptera frugiperda and the like, the control effect is better, and compared with a single medicament, the insecticidal composition has a certain synergistic effect, the insecticidal efficiency is higher, and the drug resistance is not easy to generate.
Furthermore, the insecticidal effective components of the insecticidal composition adopt chlorantraniliprole and lufenuron with the weight ratio of 5.2-6.6:11.0-12.7, compared with other mixed medicines with other proportions, the short-term insecticidal effect and the long-term insecticidal effect of the insecticidal composition are greatly improved, the overall cost is lower, and the economic benefit is remarkable. According to the application, the chlorantraniliprole and lufenuron with the weight ratio of 5.2-6.6:11.0-12.7 are used, so that the dosage of lufenuron is more, and the polyarylphenol polyether phosphate can be better combined with trifluoromethyl and other fluoroalkyl in the lufenuron, so that the lufenuron is promoted to be uniformly dispersed in water or other dispersion systems, and preparations such as a suspending agent with more uniform and stable dispersion are conveniently prepared, and the insecticidal effect is further improved.
Preferably, the insecticidal effective component further comprises a synergistic component, wherein the synergistic component is at least one of ferulic aldehyde and a ferulic aldehyde derivative product, and the weight ratio of the synergistic component to chlorantraniliprole is 1.2-1.8:5.2-6.6, wherein the ferulic aldehyde derivative product is prepared from ferulic aldehyde and phenylhydrazine.
By adopting the technical scheme, the molecular structure of the ferulic aldehyde or the ferulic aldehyde derivative product is smaller, and the molecule contains hydroxyl groups, so that the effect of sucking insect killing is realized, and the effect of sucking insect killing comprehensively by matching with chlorantraniliprole and lufenuron is realized, so that the insect killing is more thorough.
Further, the antifreezing agent is glycol, the antifoaming agent is magnesium aluminum silicate, the thickening agent is xanthan gum, and the preservative is kathon. By adopting the technical scheme, the ethylene glycol not only can improve the antifreezing performance of the pesticide and the adaptability of the pesticide to temperature, but also can improve the dispersion performance of the insecticidal effective ingredient chlorantraniliprole which is indissolvable in water and improve the dispersion uniformity degree of the insecticidal effective ingredient in water. The magnesium aluminum silicate can improve the uniform stability of the final pesticide, and can improve the adhesion capability of the pesticide on the leaf surfaces of crops together with the xanthan gum, so as to further improve the insecticidal persistence.
Further, the sodium alkyl sulfonate is at least one of sodium dodecyl sulfonate and sodium tetradecyl sulfonate. The polyarylphenol polyether phosphate is tristyrylphenol polyoxyethylene ether phosphate.
Further, the insecticidal composition is a broad-spectrum insecticidal composition with stomach toxicity and contact type. Further, the insecticidal composition is an insecticidal composition against spodoptera frugiperda. Further, the insecticidal composition is an insecticidal composition against spodoptera frugiperda.
In a second aspect, the pesticide with multiple functions provided by the application adopts the following technical scheme:
a pesticide with multiple functions is prepared from the following raw materials in percentage by weight: 16 to 21.5 percent of insecticidal active ingredient, 3.5 to 4.2 percent of sodium alkyl sulfonate, 3.0 to 4.0 percent of polyarylphenol polyether phosphate, 2.8 to 3.1 percent of antifreezing agent, 0.5 to 0.7 percent of defoaming agent, 0.1 to 0.2 percent of thickening agent, 0.1 to 0.15 percent of preservative and the balance of water; the insecticidal effective components comprise chlorantraniliprole and lufenuron in a weight ratio of 5.2-6.6:11.0-12.7.
By adopting the technical scheme, the insecticidal effective components of the insecticide are compounded by chlorantraniliprole and lufenuron, so that the insecticide has two insecticidal effects of stomach toxicity and contact killing, and the chlorantraniliprole and lufenuron have a certain synergistic effect, so that the insecticidal rate and the control effect of the insecticide are greatly improved. The chlorantraniliprole and lufenuron in the insecticidal effective components are in a weight ratio of 5.2-6.6:11.0-12.7, and the chlorantraniliprole and lufenuron are mutually promoted, so that the short-term insecticidal effect and the long-term insecticidal effect of the insecticide are improved, the lasting period of the insecticide is prolonged, and the good insecticidal effect can be ensured by lower application dosage when the insecticidal composition is used. The insecticide prepared from chlorantraniliprole and lufenuron in the weight ratio has the advantages of both insecticidal effect and economic benefit, high prevention effect and relatively low cost.
Preferably, the insecticidal effective component further comprises a synergistic component, wherein the synergistic component is at least one of ferulic aldehyde and a ferulic aldehyde derivative product, the weight ratio of the synergistic component to chlorantraniliprole is 1.2-1.8:5.2-6.6, and the ferulic aldehyde derivative product is prepared from ferulic aldehyde and phenylhydrazine.
By adopting the technical scheme, the ferulic aldehyde or the ferulic aldehyde derivative product can promote the internal absorption type insecticidal effect of the insecticide, so that the insecticidal effect of the insecticide is more comprehensive, the insecticidal control effect is further improved, and the ferulic aldehyde or the ferulic aldehyde derivative product has a certain synergistic effect with chlorantraniliprole and lufenuron after being added, and has more outstanding insecticidal effect on spodoptera frugiperda.
Preferably, the insecticidal effective components consist of chlorantraniliprole, lufenuron, ferulic aldehyde and ferulic aldehyde derivative products with the weight ratio of 5.2-6.6:11.0-12.7:0.5-0.6:1.2-1.3.
By adopting the technical scheme, the insecticidal active ingredient consists of four insecticidal active substances, the insecticidal composition can promote the insecticidal effect of the insecticide in various aspects such as stomach toxicity, contact killing and internal absorption, the synergistic effect of ferulic aldehyde and the ferulic aldehyde derivative products on chlorantraniliprole and lufenuron is more remarkable, and the insecticidal rate and the control effect of the insecticide prepared by the four substances on spodoptera frugiperda are far beyond those of the existing single insecticide and the insecticide compounded by two single medicaments.
Preferably, the preparation method of the ferulic aldehyde derivative product comprises the following steps: mixing ferulic aldehyde and phenylhydrazine in organic solvent, refluxing, cooling, crystallizing, separating solid from liquid, washing, and drying.
By adopting the technical scheme, the ferulic aldehyde derivative product is prepared by mixing and reacting ferulic aldehyde and phenylhydrazine in a solvent, and the hydrazone structure is introduced into the molecules of part of substances in the product, so that the product has a unique insecticidal effect on spodoptera frugiperda pests, and further the control effect of the insecticide is improved.
Further, acetic acid is added when ferulic aldehyde and phenylhydrazine are mixed and refluxed. The addition amount of acetic acid is 1-2mL of glacial acetic acid added to every 1.78g of ferulic aldehyde. Acetic acid can be used as a proton catalyst to improve the reaction efficiency. The solvent is at least one of methanol, ethanol, ethyl acetate and pyridine. The reflux temperature for the reaction may be set according to the type of solvent, and is generally 60 to 120℃and preferably 60 to 80 ℃. The reflux time is 5-12h. The washing solvent is methanol, ethanol or ethyl acetate. After washing, the mixture can be subjected to secondary washing by petroleum ether.
Preferably, the mass ratio of the ferulic aldehyde to the phenylhydrazine is 1.7-1.85:1-1.2.
By adopting the technical scheme, the reaction is carried out under the condition of equimolar or slightly excessive phenylhydrazine, so that the yield of the ferulic aldehyde derivative product can be improved. The amount of the organic solvent is 150mL for every 1-1.2g phenylhydrazine. When the reaction is carried out specifically, the phenylhydrazine hydrochloride with the same amount can be used for replacing phenylhydrazine to carry out the reaction, and other conditions are unchanged. The ferulic aldehyde can also be replaced by equivalent nitroferulic aldehyde for reaction, and other conditions are unchanged.
Further, the pesticide is broad-spectrum pesticide with stomach toxicity and contact type. Further, the insecticide is an insecticide against spodoptera frugiperda. Further, the insecticide is an insecticide against spodoptera frugiperda.
Further, the washing is carried out by adopting a washing solvent at the temperature of between 10 ℃ below zero and 15 ℃ below zero so as to reduce the loss of effective products.
Further, the weight percentage of the insecticidal effective components in the raw materials is 18-19.5%, and further, the weight percentage of the insecticidal effective components in the raw materials is 18%. Further, the antifreezing agent is glycol, the antifoaming agent is magnesium aluminum silicate, the thickening agent is xanthan gum, and the preservative is kathon.
In a third aspect, the method for preparing the pesticide with multiple functions provided by the application adopts the following technical scheme:
the preparation method of the pesticide with multiple functions comprises the following steps:
uniformly mixing a thickener and part of water to prepare thickener dispersion liquid;
uniformly mixing chlorantraniliprole, lufenuron, sodium alkyl sulfonate, polyarylphenol polyether phosphate, an antifreezing agent and the rest water to obtain slurry, performing sanding treatment on the slurry for 3-4h, and then adding a thickener dispersion liquid, a defoaming agent and a preservative, and performing sanding treatment to obtain the insecticidal composition.
According to the technical scheme, the dispersing uniformity of the insecticidal effective components can be improved, the insecticidal effective components such as chlorantraniliprole, lufenuron and the like are not dissolved in water, so that the insecticidal effective components are not easy to disperse uniformly in water when the suspending agent is prepared, the insecticidal effect of the insecticide is greatly reduced.
Further, the weight ratio of the water mixed with the thickener to the remaining water (water mixed with chlorantraniliprole, lufenuron, sodium alkyl sulfonate, polyarylphenol polyether phosphate, antifreeze) is 10-12:59-62. The thickener and part of water are uniformly mixed, namely the thickener and part of water are subjected to shearing dispersion for 2-2.5 hours in a high shearing dispersion emulsifying machine. The chlorantraniliprole, lufenuron, sodium alkyl sulfonate, polyaryl phenol polyether phosphate and antifreezing agent are uniformly mixed with the rest of water, and the chlorantraniliprole, lufenuron, sodium alkyl sulfonate, polyaryl phenol polyether phosphate, antifreezing agent and the rest of water are sheared for 30-45min in a high shearing dispersion emulsifying machine.
Preferably, the uniformly mixing of chlorantraniliprole, lufenuron, sodium alkyl sulfonate, polyarylphenol polyether phosphate, antifreezing agent and the rest water comprises the following steps: uniformly mixing chlorantraniliprole, an antifreezing agent and a part of the rest water to obtain chlorantraniliprole dispersion; uniformly mixing lufenuron, polyarylphenol polyether phosphate and the other part of the rest water to obtain lufenuron dispersion liquid; uniformly mixing chlorantraniliprole dispersion liquid and lufenuron dispersion liquid, then adding sodium alkyl sulfonate and the rest part of the rest water, and uniformly mixing to obtain slurry; the antifreezing agent is glycol.
By adopting the technical scheme, when chlorantraniliprole, lufenuron, sodium alkyl sulfonate, polyarylphenol polyether phosphate and antifreezing agent are uniformly mixed with the rest water, the chlorantraniliprole is firstly mixed with ethylene glycol (antifreezing agent), the amino group in the chlorantraniliprole is easier to combine with the ethylene glycol, and finally the dispersing effect of the chlorantraniliprole in the water is improved; the lufenuron contains trifluoromethyl and other fluoroalkyl groups, can be better combined with the polyarylphenol polyether phosphate, can be dispersed more uniformly when being dispersed in water, is easier to form small particles, and finally improves the uniformity of the dispersion of the insecticidal active ingredient in the water. Further, the weight ratio of the water mixed with the thickener, the water mixed with chlorantraniliprole and the antifreezing agent to the water mixed with lufenuron and the polyarylphenol polyether phosphate is 1-1.5:1-1.5:2-3. Further, the weight ratio of the water mixed with the thickener, the water mixed with chlorantraniliprole and the antifreezing agent and the water mixed with lufenuron and polyarylphenol polyether phosphate is 1:1:2. When the chlorantraniliprole, the antifreezing agent and a part of the rest water are uniformly mixed, the chlorantraniliprole and the antifreezing agent are uniformly mixed firstly and then added into the rest water for uniform mixing.
The evenly mixing of the lufenuron and the polyarylphenol polyether phosphate with the other part of the rest water is that the lufenuron and the polyarylphenol polyether phosphate are evenly mixed and then added into the other part of the rest water for evenly mixing.
Further, the sanding treatment is carried out after adding the thickener dispersion liquid, the defoamer and the preservative until the particle size of the suspended particles is not more than 5 mu m.
In a fourth aspect, the present application provides a pesticide having multiple effects, which adopts the following technical scheme:
the application of the pesticide with multiple functions in preventing and controlling corn spodoptera frugiperda.
By adopting the technical scheme, when the pesticide with multiple functions is applied to the prevention and control of the spodoptera frugiperda, the pesticide has stronger pertinence, has higher prevention and control effect on the spodoptera frugiperda and has long lasting period.
Further, the application comprises the following steps: the corn is applied from the incubation period of the spodoptera frugiperda eggs to the initial period of the low-age larva, and the application dosage is 10-30 g/mu. The application mode is spraying. The medicine is applied 1 time in each season.
In summary, the present application includes at least one of the following beneficial technical effects:
1. the insecticidal composition and the insecticide with multiple functions have the advantages that the chlorantraniliprole and the lufenuron are adopted as the insecticidal active ingredients, the chlorantraniliprole and the lufenuron can be synergistic, the insecticidal effect is better, and the polyarylphenol polyether phosphate is also added into the insecticidal composition and the insecticide, so that the chlorfenuron has good dispersion promoting effect, the insecticidal active ingredients are uniformly dispersed in water, and the insecticidal effect is further improved.
2. The pesticide with multiple functions of the application further adds ferulic aldehyde and/or ferulic aldehyde derivative products into the pesticide active ingredients, so that the pesticide has multiple pesticide effects, is more comprehensive in pesticide effect, has higher control effect, greatly improves the lasting period and also reduces the probability of drug resistance of pests.
3. When the pesticide with multiple functions is prepared, chlorantraniliprole is mixed with glycol, lufenuron is mixed with polyarylphenol polyether phosphate and then dispersed in water, so that the uniformity of the dispersion of chlorantraniliprole and lufenuron in water is improved, and the suspending agent with smaller particle size is prepared.
Detailed Description
The present application will be described in further detail with reference to examples.
Chlorantraniliprole is a benzamide broad-spectrum pesticide, and is used for controlling pests by activating a Raney receptor of a target pest, and the activation of the Raney receptor of the pest can release calcium ions stored in smooth muscle and striated muscle cells, so that muscle regulation is weakened and paralysis is caused, and the pest is killed. When chlorantraniliprole is used for killing insects, the action mode is mainly stomach toxicity. The chlorantraniliprole has very obvious selectivity difference on the Raney acceptors of mammals and pests, so that the chlorantraniliprole has higher safety on natural enemies of people and pests, and therefore, the chlorantraniliprole is widely used. However, as the application of chlorantraniliprole is more and more widespread, many pests have stronger resistance, and the popularization of the chlorantraniliprole in recent years is affected to a certain extent due to the high price of the chlorantraniliprole.
The lufenuron is a substituted urea pesticide, can inhibit the synthesis of the chitin, kills pests by acting on insect larvae and preventing the insect larvae from peeling, has good control effect on leaf-eating caterpillars of fruit trees and the like, and is suitable for controlling the pests with resistance to synthetic pyrethrins and organophosphorus pesticides. The lufenuron has the main insecticidal action mode of contact killing, can kill eggs and has remarkable control effect on piercing-sucking pests.
The applicant has carried out a great deal of researches on the prevention and treatment of spodoptera frugiperda in various existing pesticides including chlorantraniliprole and lufenuron, and as a result, the pesticide is found to be used in a compound way aiming at the stronger drug resistance of spodoptera frugiperda, and the prevention and treatment effects are improved to different degrees. For example, by mixing chlorantraniliprole and lufenuron, two medicaments with different action mechanisms can form multi-site action, so that the target is not easy to generate drug resistance, and the quick-acting and lasting effects are combined, thereby having stomach toxicity and contact killing effects. It can also enlarge the control object and delay the generation of resistance.
Based on the findings, the applicant carries out a large number of experiments on the compounding of various commercial pesticides, and the comparison of the experiment results shows that the 18% chlorantraniliprole lufenuron suspending agent has a great improvement on the control effect on spodoptera frugiperda compared with a single medicament, has better control effect compared with other compounded medicaments, and has a great improvement on the duration of the medicament.
In order to further weaken the resistance of the spodoptera frugiperda to the insecticide, the applicant also adds other insecticidal active substances to compound on the basis of chlorantraniliprole and lufenuron compound, and experiments show that the ferulic acid and the derivatives thereof have better synergistic effect on the prevention effect of the insecticide, can realize the decrement use of the insecticide and have better selectivity. After a small amount of ferulic acid derivative is added, the pesticide is relatively safe to the natural environment while ensuring high prevention effect.
Preparation example 1
The preparation method of the ferulic aldehyde derivative product comprises the following steps: adding 1.78g of ferulic aldehyde and 1g of phenylhydrazine into 150mL of ethanol, adding 1mL of glacial acetic acid, uniformly mixing, heating and refluxing for 5h, cooling and crystallizing, filtering, washing the solid with methanol at the temperature of minus 10 ℃, and drying to obtain the product.
Preparation example 2
The preparation method of the ferulic aldehyde derivative product comprises the following steps: adding 1.78g of ferulic aldehyde and 1.2g of phenylhydrazine into 150mL of ethyl acetate, adding 1mL of glacial acetic acid, uniformly mixing, heating and refluxing for 10h, cooling and crystallizing, filtering, washing the solid with ethyl acetate at the temperature of minus 15 ℃, and drying to obtain the product.
The products prepared in preparation example 1 and preparation example 2 can be separated by silica gel column chromatography, and the separated distinguishable two substances are respectively recrystallized for 3 times, so that a small amount of compounds with higher purity can be obtained. However, these higher purity compounds undergo a color change in a shorter period of time (the light yellow compound gradually darkens), presumably to oxidize the compound. Thus, the product obtained in the above preparation examples is used in the following examples directly as ferulic aldehyde derivative product without isolation and recrystallization, and if preservation is required, low temperature isolation is used.
The chlorantraniliprole and lufenuron can be pure products with the purity of 99 percent or can be raw medicines sold in the market. In the following examples, commercial crude drugs were used, wherein chlorantraniliprole had a purity of 95.3% (nominal purity 95.3%, actual purity slightly more than 95.3%) and lufenuron had a purity of 97.0%. Other raw materials are all commercial products.
Example 1
The insecticidal composition of the embodiment consists of the following components in parts by weight: 6.0g of chlorantraniliprole, 12.0g of lufenuron, 4.0g of sodium alkyl sulfonate, 3.0g of polyarylphenol polyether phosphate, 3.0g of glycol, 0.5g of magnesium aluminum silicate, 0.1g of xanthan gum and 0.1g of kathon. The sodium alkyl sulfonate is sodium dodecyl sulfonate, and the polyarylphenol polyether phosphate is tristyrylphenol polyoxyethylene ether phosphate.
The pesticide with multiple functions in the embodiment is prepared from the following raw materials in parts by weight: 6.0g of chlorantraniliprole, 12.0g of lufenuron, 4.0g of sodium alkyl sulfonate, 3.0g of polyarylphenol polyether phosphate, 3.0g of glycol, 0.5g of magnesium aluminum silicate, 0.1g of xanthan gum, 0.1g of kathon and 71.3g of water. The sodium alkyl sulfonate is sodium dodecyl sulfonate, and the polyarylphenol polyether phosphate is tristyrylphenol polyoxyethylene ether phosphate.
The preparation method of the pesticide with multiple functions comprises the following steps:
1) Adding xanthan gum into 10g of water, and performing shearing dispersion for 2 hours in a high-shearing dispersion emulsifying machine to obtain thickener dispersion liquid;
2) Mixing chlorantraniliprole, lufenuron, sodium alkyl sulfonate, polyarylphenol polyether phosphate and glycol with the rest water, adding into a high-shear dispersing emulsifying machine for shearing and dispersing for 30min, and uniformly dispersing the materials to obtain slurry;
3) Transferring the slurry into a sand mill, and performing sand milling treatment for 3 hours; then adding thickener dispersion liquid, magnesium aluminum silicate and kathon, continuing sanding, and detecting slurry in the process of continuing sanding, and stopping sanding when the particle size of suspended particles is not more than 5 mu m; and detecting the finished product after sanding, and packaging and warehousing qualified products.
The application of the pesticide with multiple functions in the embodiment comprises the following steps: the corn is applied from the incubation period of the spodoptera frugiperda eggs to the initial period of the low-age larva, and the pesticide with multiple functions is sprayed on average 12g of the pesticide with multiple functions per mu of corn by adopting a mode of diluting and spraying the pesticide with multiple functions, and the pesticide is applied for 1 time per season (crop period).
Example 2
The insecticidal composition of the embodiment consists of the following components in parts by weight: 5.5g of chlorantraniliprole, 12.5g of lufenuron, 4.0g of sodium alkyl sulfonate, 3.0g of polyarylphenol polyether phosphate, 3.0g of glycol, 0.5g of magnesium aluminum silicate, 0.1g of xanthan gum and 0.1g of kathon. The sodium alkyl sulfonate is sodium dodecyl sulfonate, and the polyarylphenol polyether phosphate is tristyrylphenol polyoxyethylene ether phosphate.
The pesticide with multiple functions in the embodiment is prepared from the following raw materials in parts by weight: 5.5g of chlorantraniliprole, 12.5g of lufenuron, 4.0g of sodium alkyl sulfonate, 3.0g of polyarylphenol polyether phosphate, 3.0g of glycol, 0.5g of magnesium aluminum silicate, 0.1g of xanthan gum, 0.1g of kathon and 71.3g of water. The sodium alkyl sulfonate is sodium dodecyl sulfonate, and the polyarylphenol polyether phosphate is tristyrylphenol polyoxyethylene ether phosphate.
The preparation method of the insecticide having multiple functions of this example is the same as that of example 1.
The application of the insecticide having multiple functions of this example is the same as that of example 1.
Example 3
The insecticidal composition of the embodiment consists of the following components in parts by weight: 6.6g of chlorantraniliprole, 11.4g of lufenuron, 4.0g of sodium alkyl sulfonate, 3.0g of polyarylphenol polyether phosphate, 3.0g of glycol, 0.5g of magnesium aluminum silicate, 0.1g of xanthan gum and 0.1g of kathon. The sodium alkyl sulfonate is sodium dodecyl sulfonate, and the polyarylphenol polyether phosphate is tristyrylphenol polyoxyethylene ether phosphate.
The pesticide with multiple functions in the embodiment is prepared from the following raw materials in parts by weight: 6.6g of chlorantraniliprole, 11.4g of lufenuron, 4.0g of sodium alkyl sulfonate, 3.0g of polyarylphenol polyether phosphate, 3.0g of glycol, 0.5g of magnesium aluminum silicate, 0.1g of xanthan gum, 0.1g of kathon and 71.3g of water. The sodium alkyl sulfonate is sodium dodecyl sulfonate, and the polyarylphenol polyether phosphate is tristyrylphenol polyoxyethylene ether phosphate.
The preparation method of the insecticide having multiple functions of this example is the same as that of example 1.
The application of the insecticide having multiple functions of this example is the same as that of example 1.
Example 4
The insecticidal composition of the embodiment consists of the following components in parts by weight: 6.6g of chlorantraniliprole, 12.7g of lufenuron, 4.0g of sodium alkyl sulfonate, 3.0g of polyarylphenol polyether phosphate, 3.0g of glycol, 0.5g of magnesium aluminum silicate, 0.1g of xanthan gum and 0.1g of kathon. The sodium alkyl sulfonate is sodium tetradecyl sulfonate, and the polyarylphenol polyether phosphate is tristyrylphenol polyoxyethylene ether phosphate.
The pesticide with multiple functions in the embodiment is prepared from the following raw materials in parts by weight: 6.6g of chlorantraniliprole, 12.7g of lufenuron, 4.0g of sodium alkyl sulfonate, 3.0g of polyarylphenol polyether phosphate, 3.0g of glycol, 0.5g of magnesium aluminum silicate, 0.1g of xanthan gum, 0.1g of kathon and 71.2g of water. The sodium alkyl sulfonate is sodium tetradecyl sulfonate, and the polyarylphenol polyether phosphate is tristyrylphenol polyoxyethylene ether phosphate.
The preparation method of the insecticide having multiple functions of this example is the same as that of example 1.
The application of the insecticide having multiple functions of this example is the same as that of example 1.
Example 5
The insecticidal composition of the embodiment consists of the following components in parts by weight: 5.5g of chlorantraniliprole, 12.5g of lufenuron, 3.5g of sodium alkyl sulfonate, 4.0g of polyarylphenol polyether phosphate, 2.8g of glycol, 0.7g of magnesium aluminum silicate, 0.2g of xanthan gum and 0.15g of kathon. The sodium alkyl sulfonate is sodium dodecyl sulfonate, and the polyarylphenol polyether phosphate is tristyrylphenol polyoxyethylene ether phosphate.
The pesticide with multiple functions in the embodiment is prepared from the following raw materials in parts by weight: 5.5g of chlorantraniliprole, 12.5g of lufenuron, 3.5g of sodium alkyl sulfonate, 4.0g of polyarylphenol polyether phosphate, 2.8g of glycol, 0.7g of magnesium aluminum silicate, 0.2g of xanthan gum, 0.15g of kathon and 70.65g of water. The sodium alkyl sulfonate is sodium dodecyl sulfonate, and the polyarylphenol polyether phosphate is tristyrylphenol polyoxyethylene ether phosphate.
The preparation method of the insecticide having multiple functions of this example is the same as that of example 1.
The application of the insecticide having multiple functions of this example is the same as that of example 1.
Example 6
The insecticidal composition of the embodiment consists of the following components in parts by weight: 5.5g of chlorantraniliprole, 12.5g of lufenuron, 1.2g of ferulic aldehyde, 4.0g of sodium alkyl sulfonate, 3.0g of polyarylphenol polyether phosphate, 3.0g of glycol, 0.5g of magnesium aluminum silicate, 0.1g of xanthan gum and 0.1g of kathon. The sodium alkyl sulfonate is sodium dodecyl sulfonate, and the polyarylphenol polyether phosphate is tristyrylphenol polyoxyethylene ether phosphate.
The pesticide with multiple functions in the embodiment is prepared from the following raw materials in parts by weight: 5.5g of chlorantraniliprole, 12.5g of lufenuron, 1.2g of ferulic aldehyde, 4.0g of sodium alkyl sulfonate, 3.0g of polyarylphenol polyether phosphate, 3.0g of glycol, 0.5g of magnesium aluminum silicate, 0.1g of xanthan gum, 0.1g of kathon and 70.1g of water. The sodium alkyl sulfonate is sodium dodecyl sulfonate, and the polyarylphenol polyether phosphate is tristyrylphenol polyoxyethylene ether phosphate.
The preparation method of the insecticide with multiple functions of this example is different from that of example 1 in that ferulic aldehyde is also added when chlorantraniliprole, lufenuron, sodium alkyl sulfonate, polyarylphenol polyether phosphate, glycol and the rest of water are mixed in step 2), otherwise the same as in example 1.
The application of the insecticide having multiple functions of this example is the same as that of example 1.
Example 7
The insecticidal composition of the embodiment consists of the following components in parts by weight: 5.5g of chlorantraniliprole, 12.5g of lufenuron, 1.2g of ferulic aldehyde derivative, 4.0g of sodium alkyl sulfonate, 3.0g of polyarylphenol polyether phosphate, 3.0g of glycol, 0.5g of magnesium aluminum silicate, 0.1g of xanthan gum and 0.1g of kathon. The ferulic aldehyde derivative was the ferulic aldehyde derivative prepared in preparation example 1. The sodium alkyl sulfonate is sodium dodecyl sulfonate, and the polyarylphenol polyether phosphate is tristyrylphenol polyoxyethylene ether phosphate.
The pesticide with multiple functions in the embodiment is prepared from the following raw materials in parts by weight: 5.5g of chlorantraniliprole, 12.5g of lufenuron, 1.2g of ferulic aldehyde derivative product, 4.0g of sodium alkyl sulfonate, 3.0g of polyarylphenol polyether phosphate, 3.0g of glycol, 0.5g of magnesium aluminum silicate, 0.1g of xanthan gum, 0.1g of kathon and 70.1g of water. The ferulic aldehyde derivative was the ferulic aldehyde derivative prepared in preparation example 1. The sodium alkyl sulfonate is sodium dodecyl sulfonate, and the polyarylphenol polyether phosphate is tristyrylphenol polyoxyethylene ether phosphate.
The preparation method of the insecticide with multiple functions of this example is different from that of example 1 in that the chlorantraniliprole, lufenuron, sodium alkyl sulfonate, polyarylphenol polyether phosphate, glycol and the rest of water are mixed in step 2), and ferulic aldehyde derivative product is also added, otherwise the same as in example 1.
The application of the insecticide having multiple functions of this example is the same as that of example 1.
Example 8
The insecticidal composition of this example was different from the insecticidal composition of example 7 in that the weight of the ferulic aldehyde-derived product was 1.8g, and otherwise the same as in example 7.
The multi-acting insecticide of this example was different from the multi-acting insecticide of example 7 in that the weight of the ferulic aldehyde-derived product was 1.8g, the weight of water was 69.5g, and otherwise the same as in example 7.
The preparation method of the insecticide having multiple functions of this example is the same as that of example 7.
The application of the insecticide having multiple functions of this example is the same as that of example 7.
Example 9
The insecticidal composition of this example was different from the insecticidal composition of example 7 in that the weight of the ferulic aldehyde-derived product was 1.5g, and otherwise the same as in example 7.
The multi-acting insecticide of this example was different from the multi-acting insecticide of example 7 in that the weight of the ferulic aldehyde-derived product was 1.5g, the weight of water was 69.8g, and otherwise the same as in example 7.
The preparation method of the insecticide having multiple functions of this example is the same as that of example 7.
The application of the insecticide having multiple functions of this example is the same as that of example 7.
Example 10
The insecticidal composition of this example was different from the insecticidal composition of example 9 in that 0.6g of ferulic aldehyde and 1.2g of ferulic aldehyde-derived product were used instead of 1.5g of ferulic aldehyde-derived product, and the other was the same as in example 9.
The multi-acting insecticide of this example was different from the multi-acting insecticide of example 9 in that 0.6g of ferulic aldehyde and 1.2g of ferulic aldehyde-derived product were used instead of 1.5g of ferulic aldehyde-derived product, and the other was the same as in example 9.
The preparation method of the insecticide having multiple effects of this example is different from that of example 9 in that ferulic aldehyde is added along with the ferulic aldehyde derivative.
The application of the insecticide having multiple functions of this example is the same as that of example 9.
Example 11
The insecticidal composition of this example was different from the insecticidal composition of example 10 in that chlorantraniliprole was 5.2g in weight, lufenuron was 11.0g in weight, ferulic aldehyde was 0.6g in weight, and ferulic aldehyde-derived product was 1.2g in weight, except that the other was the same as in example 10.
The pesticide with multiple functions of this example was different from the pesticide with multiple functions of example 10 in that chlorantraniliprole was 5.2g in weight, lufenuron was 11.0g in weight, ferulic aldehyde was 0.6g in weight, ferulic aldehyde-derived product was 1.2g in weight, and water was 71.3g in weight, otherwise the same as in example 10.
The preparation method of the insecticide having multiple functions of this example is the same as that of example 10.
The application of the insecticide having multiple functions of this example was the same as that of example 10.
Example 12
The insecticidal composition of this example and the insecticide having multiple functions are different from the insecticidal composition of example 11 and the insecticide having multiple functions in that the ferulic aldehyde-derived product was the ferulic aldehyde-derived product prepared in preparation example 2.
The other components are the same as those in example 11.
Example 13
The insecticidal composition of this example and the insecticide having multiple effects are the same as in example 1.
The preparation method of the pesticide with multiple functions comprises the following steps:
1) Adding xanthan gum into 10g of water, and performing shearing dispersion for 2.5 hours in a high-shearing dispersion emulsifying machine to obtain thickener dispersion liquid; stirring and mixing chlorantraniliprole and glycol uniformly, adding 10g of water, mixing, transferring into a high-shear dispersing emulsifying machine, and shearing and dispersing for 5min to obtain chlorantraniliprole dispersion;
uniformly stirring and mixing lufenuron and polyarylphenol polyether phosphate, then adding 20g of water for mixing, and transferring into a high-shear dispersing emulsifying machine for shearing and dispersing for 10min to obtain lufenuron dispersion liquid;
2) Adding the chlorantraniliprole dispersion liquid and lufenuron dispersion liquid prepared in the step 1) into a high-shear dispersing emulsifying machine for shearing and dispersing for 2min, then adding sodium alkyl sulfonate and the rest of water, and then carrying out high-speed shearing and dispersing for 5min to obtain slurry;
3) Transferring the slurry into a sand mill, and performing sand milling treatment for 3.5 hours; then adding the thickener dispersion liquid, magnesium aluminum silicate and pinocembrane, and continuing sanding. In the process of continuing the sanding treatment, the slurry is taken for detection, and the sanding is stopped when the particle size of the suspended particles is detected to be not more than 5 mu m; and detecting the finished product after sanding, and packaging and warehousing qualified products.
Comparative example 1
The insecticidal composition of this comparative example was different from the insecticidal composition of example 1 in that 18.0g of chlorantraniliprole was used instead of 6.0g of chlorantraniliprole and 12.0g of lufenuron in example 1, and the other was the same as in example 1.
The insecticide of this comparative example was different from the insecticide of example 1 in that 18.0g of chlorantraniliprole was used instead of 6.0g of chlorantraniliprole and 12.0g of lufenuron in example 1, and the other was the same as in example 1.
The preparation method of the insecticide of this comparative example was referred to the preparation method in example 1.
Comparative example 2
The insecticidal composition of this comparative example was different from the insecticidal composition of example 1 in that 5.5g of chlorantraniliprole was used instead of 6.0g of chlorantraniliprole and 12.0g of lufenuron in example 1, and the other was the same as in example 1.
The insecticide of this comparative example was different from the insecticide of example 1 in that 5.5g of chlorantraniliprole was used instead of 6.0g of chlorantraniliprole and 12.0g of lufenuron in example 1, and the other was the same as in example 1.
The preparation method of the insecticide of this comparative example was referred to the preparation method in example 1.
Comparative example 3
The insecticidal composition of this comparative example was different from the insecticidal composition of example 1 in that 18.0g of lufenuron was used instead of 6.0g of chlorantraniliprole and 12.0g of lufenuron in example 1, and the other was the same as in example 1.
The insecticide of this comparative example was different from the insecticide of example 1 having multiple functions in that 18.0g of lufenuron was used instead of 6.0g of chlorantraniliprole and 12.0g of lufenuron in example 1, and the other was the same as in example 1.
The preparation method of the insecticide of this comparative example was referred to the preparation method in example 1.
Comparative example 4
The insecticidal composition of this comparative example was different from the insecticidal composition of example 1 in that 12.5g of lufenuron was used instead of 6.0g of chlorantraniliprole and 12.0g of lufenuron in example 1, and the other was the same as in example 1.
The insecticide of this comparative example was different from the insecticide of example 1 having multiple functions in that 12.5g of lufenuron was used instead of 6.0g of chlorantraniliprole and 12.0g of lufenuron in example 1, and the other was the same as in example 1.
The preparation method of the insecticide of this comparative example was referred to the preparation method in example 1.
Comparative example 5
The insecticidal composition of this comparative example was different from the insecticidal composition of example 1 in that chlorantraniliprole had a weight of 3.2g and lufenuron had a weight of 8.8g, and the other was the same as in example 1.
The insecticide of this comparative example was different from the insecticide of example 1 in that chlorantraniliprole was 3.2g in weight, lufenuron was 8.8g in weight, and water was 77.3g in weight, otherwise the same as in example 1.
The preparation method of the insecticide of this comparative example was referred to the preparation method in example 1.
Comparative example 6
The insecticidal composition of this comparative example was different from the insecticidal composition of example 1 in that 0.6g of ferulic aldehyde was used instead of 6.0g of chlorantraniliprole and 12.0g of lufenuron in example 1, and the other was the same as in example 1.
The insecticide of this comparative example was different from the insecticide of example 1 having multiple effects in that 0.6g of ferulic aldehyde was used instead of 6.0g of chlorantraniliprole and 12.0g of lufenuron in example 1, and the other was the same as in example 1.
The preparation method of the insecticide of this comparative example was referred to the preparation method in example 1.
Comparative example 7
The insecticidal composition of this comparative example was different from the insecticidal composition of example 1 in that 1.2g of ferulic aldehyde-derived product was used instead of 6.0g of chlorantraniliprole and 12.0g of lufenuron in example 1, the ferulic aldehyde-derived product being the ferulic aldehyde-derived product produced in preparation example 1, and the other being the same as in example 1.
The pesticide of this comparative example was different from the pesticide of example 1 in that 1.2g of ferulic aldehyde-derived product, which was the ferulic aldehyde-derived product produced in preparation example 1, was used instead of 6.0g of chlorantraniliprole and 12.0g of lufenuron in example 1, and the other was the same as in example 1.
The preparation method of the insecticide of this comparative example was referred to the preparation method in example 1.
Comparative example 8
The insecticidal composition of this comparative example was different from the insecticidal composition of example 1 in that 7.0g of sodium alkyl sulfonate was used instead of 4.0g of sodium alkyl sulfonate and 3.0g of polyarylphenol polyether phosphate in example 1, and the other was the same as in example 1.
The pesticide of this comparative example was different from the pesticide of example 1 in that 7.0g of sodium alkyl sulfonate was used instead of 4.0g of sodium alkyl sulfonate and 3.0g of polyarylphenol polyether phosphate in example 1, and the other was the same as in example 1.
The preparation method of the insecticide of this comparative example was referred to the preparation method in example 1.
Performance test
1. Test of insecticidal Effect
Selecting a piece of corn-planted test field, wherein the corn is in a seedling stage. After treatment, statistics show that the density of the insect population of spodoptera frugiperda is about 17 per hundred plants, the insect plant rate is about 12%, and a field pesticide effect test is carried out on the corn field. In the test, corn fields are divided into test cells with the size of 5m by 6m, and then each cell is sprayed with a medicament.
The pesticides in examples 1-12 and comparative examples 1-7 were sprayed in different communities, respectively, and the pesticide was diluted with clear water during spraying to ensure that the spraying amount was 12 g/mu. The environmental conditions during spraying are as follows: the temperature is 18-25 ℃, the relative humidity of air is about 60%, and the wind speed is less than 4m/s.
Clear water was used as a blank.
And counting the insecticidal conditions on the 1 st day, the 3 rd day and the 7 th day after the application, and calculating the reduction rate of insect population and the prevention and treatment effect according to the following formula.
Rate of reduction of insect population = (number of insect population before control-number of insect population after control) ×100%/number of insect population before control
Control effect = (PT rate of reduction of insect population-CK rate of reduction of insect population)/(100-CK rate of reduction of insect population)
Wherein, the PT rate of reduction of insect population is the rate of reduction of insect population of the district treated by the insecticide, and the CK rate of reduction of insect population is the rate of reduction of insect population of the control district treated by the clean water.
The test results are shown in Table 1.
TABLE 1 control effects of the insecticides in examples 1 to 12 and comparative examples 1 to 7
Note that: * Data anomalies, which may be related to lower spray levels (12 g/mu) used in the test and lower concentrations of agent used in the cell, were only referenced.
* Data are abnormal, the spraying amount (12 g/mu) is low in the cell test, and the concentration of the adopted medicament is too low, so that the insecticidal effect is poor.
* Data were abnormal, the amount of spray (12 g/mu) was low in the cell test, and the concentration of the agent used was also low, data were only used as reference.
(1) According to the examples 1-3, the comparative example 1 and the comparative example 3 and the contents of the tables, when the pesticide with multiple functions is used for controlling spodoptera frugiperda, the chlorantraniliprole and lufenuron are compounded, and the reduction rate of the insect population and the control effect are both greater than those of the chlorantraniliprole and lufenuron single agent with the same dosage, which indicates that the combination of the chlorantraniliprole and lufenuron greatly improves the control effect on spodoptera frugiperda.
According to comparative example 2, comparative example 4, and in combination with the contents of the above table, the theoretical rate of reduction of the insect population of the chlorantraniliprole and lufenuron formulation was calculated according to the following formula, using the data of reduction of the insect population on the first day:
E=(X1+X2)-X1*X2/100
wherein X1 and X2 are the rate of reduction of the insect population of the insecticide of comparative example 2 and comparative example 4, respectively. In calculation, it is default that the auxiliaries other than the insecticidal effective ingredient have no insecticidal effect.
The calculation shows that the theoretical rate of reduction of the insect population is 72.68%.
Theoretical rate of reduction of insect population-actual rate of reduction of insect population (example 2) = 72.68% -74.19% = -1.51%.
Therefore, the chlorantraniliprole and lufenuron are compounded for use, and the chlorantraniliprole and lufenuron have a certain synergistic effect.
(2) From examples 3 and 4, in combination with the contents of the above table, the first day reduction of the insect population of the insecticide of example 4 was slightly greater than that of example 3, indicating that the rapid insecticidal effect was more pronounced when the amount of chlorantraniliprole was greater than that of lufenuron, which may be related to the insecticidal pattern of chlorantraniliprole and lufenuron.
According to examples 1 to 3 and comparative example 5, in combination with the contents of the above table, when the amounts of chlorantraniliprole and lufenuron were reduced, the insecticidal effect was lowered to some extent, and thus the present application maintained the amount of the insecticidal effective ingredient at 18%.
(3) According to examples 2 and 6 in combination with the above table, when ferulic aldehyde was added to the insecticide of example 6, the rate of reduction of the insect population on the first day was not as high as that of the insecticide of example 2 on the first day, but on the 7 th day, the rate of reduction of the insect population of the insecticide of example 6 was higher than that of example 2, which indicates that the long-acting insecticidal effect of the compound insecticide was significantly improved after ferulic aldehyde was added.
According to comparative example 2, comparative example 4, comparative example 6, and in combination with the contents of the above table, the theoretical reduction rate of chlorantraniliprole, lufenuron, ferulic aldehyde formulation was calculated according to the following formula, using the reduction rate data of the first day:
E=X1+X2+X3-[(X1*X2+X1*X3+X2*X3)/100+X1*X2*X3/10000]
Wherein X1, X2 and X3 are the rate of reduction of the insect population of the insecticide of comparative examples 2, 4 and 6, respectively. In calculation, it is default that the auxiliaries other than the insecticidal effective ingredient have no insecticidal effect.
The calculation shows that the theoretical reduction rate of the insect population is 73.50 percent.
Theoretical rate of reduction of insect population-actual rate of reduction of insect population (example 6) =73.50% -72.73% =0.77%.
Since the dosage of ferulic aldehyde added in example 6 is greater than that of comparative example 6 and the rate of reduction of insect population of the insecticide of example 6 is less than that of theoretical insect population, it is presumed that ferulic aldehyde has no synergistic effect when chlorantraniliprole and lufenuron ferulic aldehyde are compounded for use.
(4) According to the results of example 2 and example 7 and the contents of the tables, after the ferulic aldehyde derivative product is added into the pesticide, the reduction rate of the insect population and the prevention effect are improved to a large extent, and particularly, the reduction rate of the insect population on the 7 th day is improved to a large extent, which shows that the ferulic aldehyde can improve the long-acting insecticidal effect of the pesticide.
According to comparative example 2, comparative example 4, comparative example 7, and in combination with the contents of the above table, the theoretical reduction rate of chlorantraniliprole, lufenuron, ferulic aldehyde derivative compound was calculated according to the following formula, using the reduction rate data of the first day: e=x1+x2+x3- [ (x1×x2+x1×x3+x2×x3)/100+x1×x2×3/10000]
Wherein X1, X2 and X3 are the rate of reduction of the insect population of the insecticide of comparative example 2, comparative example 4 and comparative example 7, respectively. In calculation, it is default that the auxiliaries other than the insecticidal effective ingredient have no insecticidal effect.
The calculation shows that the theoretical reduction rate of the insect population is 76.44%.
Theoretical rate of reduction of insect population-actual rate of reduction of insect population (example 7) =76.44% -79.31% = -2.87%.
Therefore, the chlorantraniliprole, lufenuron and ferulic aldehyde derivative product compound has a certain synergistic effect.
(5) From examples 7, 8, 9, in combination with the above table, it is seen that the effect of the added amount of the ferulic aldehyde derived product on the reduction rate of the first day was not significant when the chlorantraniliprole, lufenuron and ferulic aldehyde derived product were compounded. And the comparison of the reduction rate of the insect population on the 7 th day shows that the addition amount of the ferulic aldehyde derivative product is increased, and the reduction rate of the insect population on the 7 th day is slightly improved.
(6) According to the embodiment 7 and the embodiment 10 and combining the contents of the table, when chlorantraniliprole, lufenuron, ferulic aldehyde and ferulic aldehyde derivative products are adopted for compounding, the rate of reduction of insect population on the 1 st day, the 3 rd day and the 7 th day is obviously improved compared with that of the chlorantraniliprole, lufenuron and ferulic aldehyde derivative products. Also, according to example 8 and example 10 in combination with the contents of the above table, when chlorantraniliprole, lufenuron, ferulic aldehyde and ferulic aldehyde derivative products are used for compounding, the sum of the added amounts of ferulic aldehyde and ferulic aldehyde derivative products in example 10 is the same as that of ferulic aldehyde derivative products in example 8, and the insecticide of example 10 also has a better insecticidal effect.
According to comparative example 2, comparative example 4, comparative example 6, comparative example 7, and in combination with the contents of the above table, the theoretical rate of reduction of the insect population of chlorantraniliprole, lufenuron, ferulic aldehyde derivative product formulation was calculated according to the following formula, using the first day rate of reduction of the insect population data:
E=100-(100-X1)*(100-X2)*(100-X3)*(100-X4)/1000000
wherein X1, X2, X3, X4 are the rate of reduction of the insect population of the insecticide of comparative example 2, comparative example 4, comparative example 6, comparative example 7, respectively. In calculation, it is default that the auxiliaries other than the insecticidal effective ingredient have no insecticidal effect.
The calculation shows that the theoretical reduction rate of the insect population is 77.15 percent.
Theoretical rate of reduction of insect population-actual rate of reduction of insect population (example 10) =77.15% -81.25% = -4.1%.
Therefore, the chlorantraniliprole, lufenuron, ferulic aldehyde and ferulic aldehyde derivative products have very obvious synergistic effect.
(7) From example 1, comparative example 8, and the contents of the above tables, it is understood that the reduction in the rate of reduction in the insect population of the insecticide is slightly reduced, mainly the short-term insecticidal effect is reduced, when the polyarylphenol polyether phosphate is not used, which may be related to the uniformity of dispersion of the active ingredient in the insecticide.
In summary, the pesticide provided by the application is compounded by chlorantraniliprole, lufenuron, ferulic aldehyde and ferulic aldehyde derivative products, so that the insecticidal effect of the traditional pesticide chlorantraniliprole and lufenuron is greatly improved, and most importantly, after the ferulic aldehyde and ferulic aldehyde derivative products are added, the lasting effect of the pesticide is obviously improved, the lasting period is prolonged, and the control effect is more remarkable for pests with strong reproductive capacity such as spodoptera litura on corn.
In addition, according to examples 10 and 11 in combination with the contents of the above table, in the case where the amounts of chlorantraniliprole and lufenuron in example 11 were slightly reduced, the rate of reduction of the insect population was slightly reduced as compared with example 10, but the rate of reduction of the insect population and the control effect were hardly different at day 7. Thus, after comparing the cost and control efficiency together, the applicant prepared the insecticide of example 11 as a special insecticide for controlling spodoptera frugiperda at 18% chlorpyri.
2. Testing of physical Properties of pharmaceutical Agents
Taking the pesticides in the examples 1, 13 and 8, and testing the suspension rate of the pesticides according to the test method in GB/T14825-2006 method for testing suspension rate of pesticides; and the viscosity of the insecticide was measured using a rotational viscometer (30 ℃ C., 30 r/min) and the measurement results are shown in Table 2.
TABLE 2 suspension Rate of insecticide in examples 1 and 13 and comparative example 8
Example 1 Example 13 Comparative example 8
Suspension percentage (%) 92 95 88
Viscosity (mPas) 305 313 301
According to examples 1, 13 and 8 in combination with Table 2, it is understood that the polyarylphenol polyether phosphate can promote the uniformity of dispersion of the insecticidal active ingredient in water, increase the suspension rate of the insecticide, and ensure the insecticide to have a proper viscosity. The active ingredients of the insecticide with higher suspension rate can be adhered to the leaf surface more uniformly, which is beneficial to improving the rate of reduction of insect population.

Claims (4)

1. An insecticidal composition for spodoptera frugiperda is characterized by comprising the following components in parts by weight: 16-21.5 parts of insecticidal active ingredient, 3.5-4.2 parts of sodium alkyl sulfonate, 3.0-4.0 parts of polyarylphenol polyether phosphate, 2.8-3.1 parts of antifreezing agent, 0.5-0.7 part of defoaming agent, 0.1-0.2 part of thickening agent and 0.1-0.15 part of preservative;
the insecticidal effective components consist of chlorantraniliprole, lufenuron, ferulic aldehyde and ferulic aldehyde derivative products with the weight ratio of 5.2-6.6:11.0-12.7:0.5-0.6:1.2-1.3;
the preparation method of the ferulic aldehyde derivative product comprises the following steps: mixing ferulic aldehyde and phenylhydrazine in an organic solvent, refluxing, cooling, crystallizing, separating solid from liquid, washing, and drying to obtain the final product;
the mass ratio of the ferulic aldehyde to the phenylhydrazine is 1.7-1.85:1-1.2;
acetic acid is also added when the ferulic aldehyde and the phenylhydrazine are mixed and refluxed, and the addition amount of the acetic acid is 1-2mL of glacial acetic acid added for every 1.78g of ferulic aldehyde; the reflux temperature is 60-120 ℃.
2. The pesticide with multiple functions for spodoptera frugiperda is characterized by being prepared from the following raw materials in percentage by weight: 16 to 21.5 percent of insecticidal active ingredient, 3.5 to 4.2 percent of sodium alkyl sulfonate, 3.0 to 4.0 percent of polyarylphenol polyether phosphate, 2.8 to 3.1 percent of antifreezing agent, 0.5 to 0.7 percent of defoaming agent, 0.1 to 0.2 percent of thickening agent, 0.1 to 0.15 percent of preservative and the balance of water;
The insecticidal effective components consist of chlorantraniliprole, lufenuron, ferulic aldehyde and ferulic aldehyde derivative products with the weight ratio of 5.2-6.6:11.0-12.7:0.5-0.6:1.2-1.3;
the preparation method of the ferulic aldehyde derivative product comprises the following steps: mixing ferulic aldehyde and phenylhydrazine in an organic solvent, refluxing, cooling, crystallizing, separating solid from liquid, washing, and drying to obtain the final product;
the mass ratio of the ferulic aldehyde to the phenylhydrazine is 1.7-1.85:1-1.2;
acetic acid is also added when the ferulic aldehyde and the phenylhydrazine are mixed and refluxed, and the addition amount of the acetic acid is 1-2mL of glacial acetic acid added for every 1.78g of ferulic aldehyde; the reflux temperature is 60-120 ℃.
3. A method of preparing a multi-acting insecticide against spodoptera frugiperda as claimed in claim 2 comprising the steps of:
uniformly mixing a thickener and part of water to prepare thickener dispersion liquid;
uniformly mixing chlorantraniliprole, lufenuron, sodium alkyl sulfonate, polyarylphenol polyether phosphate and antifreezing agent with the rest water to obtain slurry, performing sanding treatment on the slurry for 3-4h, then adding thickener dispersion liquid, defoamer and preservative, and performing sanding treatment to obtain the compound pesticide;
when chlorantraniliprole, lufenuron, sodium alkyl sulfonate, polyarylphenol polyether phosphate and antifreezing agent are mixed with the rest water, ferulic aldehyde and ferulic aldehyde derivative products are also added.
4. Use of a pesticide of claim 2 having multiple action against spodoptera frugiperda for controlling spodoptera frugiperda.
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