CN110150296B - Insecticidal composition of tolfenpyrad and spirotetramat and preparation method and application thereof - Google Patents

Insecticidal composition of tolfenpyrad and spirotetramat and preparation method and application thereof Download PDF

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CN110150296B
CN110150296B CN201910491573.1A CN201910491573A CN110150296B CN 110150296 B CN110150296 B CN 110150296B CN 201910491573 A CN201910491573 A CN 201910491573A CN 110150296 B CN110150296 B CN 110150296B
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spirotetramat
tolfenpyrad
insecticidal composition
agent
emulsifier
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CN110150296A (en
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袁良国
王金刚
张立滨
常建霞
魏秀国
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Qingdao Runnong Chemical 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
    • A01N25/00Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
    • A01N25/02Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing liquids as carriers, diluents or solvents
    • A01N25/04Dispersions, emulsions, suspoemulsions, suspension concentrates or gels
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N43/00Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/48Biocides, 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
    • 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
    • A01N47/02Biocides, 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 no bond to a nitrogen atom
    • A01N47/06Biocides, 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 no bond to a nitrogen atom containing —O—CO—O— groups; Thio analogues thereof

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  • Life Sciences & Earth Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Dentistry (AREA)
  • Plant Pathology (AREA)
  • Engineering & Computer Science (AREA)
  • Pest Control & Pesticides (AREA)
  • Agronomy & Crop Science (AREA)
  • Wood Science & Technology (AREA)
  • Zoology (AREA)
  • Environmental Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Dispersion Chemistry (AREA)
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  • Agricultural Chemicals And Associated Chemicals (AREA)

Abstract

The invention discloses a tolfenpyrad-spirotetramat insecticidal composition and a preparation method and application thereof, wherein the tolfenpyrad accounts for 10-40wt% of the insecticidal composition, and the spirotetramat accounts for 5-25wt% of the insecticidal composition. The invention compounds tolfenpyrad and spirotetramat to prepare the dispersible oil suspending agent, has obviously improved insecticidal effect, can be widely used for fruit and vegetable crops such as cucumbers, peppers, tomatoes, oranges, pears and the like, and can prevent and treat pests such as whitefly, aphids, psyllids, plant hoppers, scale insects, thrips, red spiders and the like of the crops. The dispersible oil suspending agent has good emulsifying dispersibility, high suspension rate and good heat storage stability, is not easy to thicken or bottom-forming, can be used for conventional spraying and spraying of a plant protection unmanned aerial vehicle, and has the advantages of difficult volatilization of liquid medicine, drift resistance, strong wetting spreadability, good permeation conductivity, rain wash resistance and high bioactivity to targets.

Description

Insecticidal composition of tolfenpyrad and spirotetramat and preparation method and application thereof
Technical Field
The invention relates to an insecticidal composition obtained by compounding tolfenpyrad and spirotetramat, and also relates to a dispersible oil suspending agent formulation of the tolfenpyrad and spirotetramat insecticidal composition, a preparation method and application thereof, belonging to the technical field of pesticides.
Background
Tolfenpyrad belongs to pyrazole amide insecticides, and the action mechanism is to block an electron transfer system complex I in a mitochondrial metabolic system, so that electron transfer is blocked. The tolfenpyrad is mainly contact-killed, has no systemic property, has long lasting period, has the functions of killing ova, inhibiting food and inhibiting oviposition, has wide insecticidal spectrum, has higher control effect on various lepidoptera, hemiptera, hymenoptera, diptera and mites, and is widely used for controlling pests of vegetables, fruit trees, flowers, tea trees, ornamental plants and the like.
Spirotetramat belongs to tetronic acid compounds, is a lipid synthesis inhibitor, and causes poisoning and death by inhibiting the synthesis of insect lipid. The spirotetramat has good two-way internal absorption and conduction performance, and can be conducted upwards through the xylem and phloem of the plant or from top to bottom in the plant. The spirotetramat has a wide insecticidal spectrum and a long persistent period, and is widely used for controlling pests such as cotton, soybeans, potatoes, tomatoes, cucumbers, eggplants, cabbages, strawberries, hot peppers, grapes, pears, oranges, bananas and the like.
The pests with piercing-sucking mouthparts such as aphids, whiteflies, psyllids, thrips, red spiders, scale insects and the like have the characteristics of short reproduction period, large reproduction quantity, obvious generation overlapping and the like, are easy to generate drug resistance, have small insect bodies, are difficult to attach on the insect bodies during medicament prevention in production, and need to be additionally added with special spraying aids. The effective component particles of dispersible oil suspending agent (OD) and its adjuvant can be stably dispersed in non-aqueous liquid, and can be diluted with water for use. The dispersible oil suspending agent selects oil auxiliary agents with good adhesiveness and spreadability as dispersing and diluting carriers, and is easy to adhere to waxy or smooth leaf surfaces, so that the dispersible oil suspending agent has the advantages of good adhesiveness and spreadability, strong permeation conductivity, strong rain erosion resistance and the like when in use, and is beneficial to the attachment of liquid medicine on insect bodies.
The pesticide variety containing a single active component has the defects that pests are easy to generate drug resistance after continuous use, the use frequency is high, the environmental pollution is aggravated and the like in the aspect of agricultural pest control, and the defects can be effectively overcome by compounding the active components with different action mechanisms. Meanwhile, the synergistic effect generated by mixing the two active components can improve the control effect, delay the generation of drug resistance of pests and reduce environmental pollution, and is an important means for comprehensively controlling the pests. At present, no report related to tolfenpyrad and spirotetramat dispersible oil suspending agents is found.
Disclosure of Invention
Aiming at the defects of poor insecticidal effect, easy generation of drug resistance and the like of single use of tolfenpyrad and spirotetramat, the invention provides the insecticidal composition of tolfenpyrad and spirotetramat, which is prepared by compounding tolfenpyrad and spirotetramat according to a specific proportion, so that a good synergistic effect is achieved, the insecticidal effect is improved, and the generation of drug resistance of pests is delayed.
The invention provides an insecticidal composition of tolfenpyrad and spirotetramat, which comprises the effective components of tolfenpyrad and spirotetramat, wherein the tolfenpyrad accounts for 10-40wt% of the insecticidal composition, and the spirotetramat accounts for 5-25wt% of the insecticidal composition.
Furthermore, the total content of the effective components in the insecticidal composition is 15-50wt%, namely the total content of the tolfenpyrad and the spirotetramat in the insecticidal composition is 15-50 wt%.
Furthermore, the mass ratio of tolfenpyrad to spirotetramat is 1-4:1, and the compounding of tolfenpyrad and spirotetramat has a better synergistic effect within the mass ratio range. Preferably, the synergistic effect is more prominent when the content of the tolfenpyrad is 30wt% and the content of the spirotetramat is 10 wt%.
In addition, aiming at the conditions that the insect body of the piercing-sucking mouthpart pests is small and the pesticide is difficult to adhere to influence the insecticidal effect, the tolfenpyrad and the spirotetramat are prepared into the dispersible oil suspending agent, and the dispersible oil suspending agent can increase the adhesiveness of liquid medicine and improve the insecticidal effect. However, in the research, the defects of high processing difficulty and poor stability of the dispersible oil suspending agent prepared from tolfenpyrad and spirotetramat are found, and aiming at the problem, the inventor conducts a large amount of screening work on an auxiliary agent system through research and a large amount of experiments to finally obtain the auxiliary agent system with good matching degree, stable performance and good insecticidal effect. Through the selection of the auxiliary agents, particularly the screening and combination of 3 auxiliary agent components of the emulsifier, the wetting agent and the stabilizer, the processing difficulty of the preparation form is greatly reduced, the stability of the preparation form is improved, the finally obtained dispersible oil suspending agent has the advantages of good emulsifying dispersibility, high suspension rate, good heat storage stability and the like, and the problems of oil precipitation or caking, flocculation, particle size growth and the like in sample storage are effectively solved.
Further, the emulsifier is one or more of alkylphenol formaldehyde resin polyoxyethylene ether, castor oil polyoxyethylene ether, phenethyl phenol polyoxyethylene polyoxypropylene ether, calcium dodecyl benzene sulfonate, sorbitan monostearate, alkylphenol polyoxyethylene ether and polyoxyethylene ether.
Furthermore, the dispersant of the invention is one or more of calcium lignosulphonate, sodium naphthalene sulfonate formaldehyde condensate, dioctyl sodium sulfosuccinate, sodium dodecyl benzene sulfonate and sodium polycarboxylate. The sodium salt of polycarboxylic acid used in the present invention may be styrene-sodium methacrylate copolymer or sodium polyacrylate.
Furthermore, the wetting agent is one or more of sodium dodecyl sulfate, sodium salt of succinic acid half ester sulfonate which is a formaldehyde condensation product of alkylphenol ethoxylates, sodium lauryl ether sulfate, sodium dodecyl sulfate and nekal BX.
Further, the thickening agent of the invention is one or more of fumed silica, polyvinyl alcohol, organic bentonite, xanthan gum and magnesium aluminum silicate.
Further, the stabilizer of the invention is one or more of tributyl phosphate, butyl hydroxy anisole, triphenyl phosphite and sodium benzoate.
Furthermore, the dispersion medium is one or more of palm oil, epoxidized soybean oil, methyl oleate, corn oil and castor oil, and the dispersion medium used in the invention is an environment-friendly solvent, so that the environment is protected, the compatibility of the components is good, and the stability of the product is improved.
Furthermore, when the auxiliary agent is optimized, the optimization of the performance of the preparation form and the drug effect of the active ingredient are more facilitated, and especially, the optimization of the emulsifying agent, the wetting agent and the stabilizing agent has better promotion effect on the performance and the drug effect of the preparation form. Preferably, the emulsifier is prepared by mixing alkylphenol formaldehyde resin polyoxyethylene ether (agricultural milk 700) and sorbitan monostearate (span 60) according to the mass ratio of 1-3: 1. Preferably, the dispersing agent is formed by mixing calcium lignosulfonate and sodium dodecyl benzene sulfonate according to the mass ratio of 1-4: 1. Preferably, the wetting agent is prepared by mixing sodium salt of alkylphenol polyoxyethylene ether formaldehyde condensate succinic acid half ester sulfonate (CAS number: 127-39-9) and nekal BX according to the mass ratio of 1: 1-3. Preferably, the thickening agent is formed by mixing fumed silica and organic bentonite according to the mass ratio of 1: 1-4. Preferably, the stabilizer is butylated hydroxyanisole. Preferably, the dispersing medium is methyl oleate.
Further, the invention provides a preferable formula of the dispersible oil suspending agent, which consists of effective components and auxiliary agents, wherein the weight percentages of the effective components and the auxiliary agents are as follows: 10-40% of tolfenpyrad, 5-25% of spirotetramat, 5-25% of emulsifier, 2-10% of dispersant, 2-8% of wetting agent, 1-6% of thickening agent, 1-5% of stabilizing agent and the balance of dispersion medium being 100%.
Further, the dispersible oil suspending agent consists of the following effective components and auxiliary agents in percentage by weight: 15-50% of active ingredients, 10-20% of emulsifier, 3-8% of dispersant, 3-6% of wetting agent, 2-5% of thickening agent, 2-4% of stabilizer and the balance of dispersion medium to 100%. Under the content of the effective components and the auxiliary agents, the components are more stable in the system and have better drug effect.
Further, the dispersible oil suspending agent consists of the following effective components and auxiliary agents in percentage by weight: 30% of tolfenpyrad, 10% of spirotetramat, 10-20% of emulsifier, 3-8% of dispersant, 3-6% of wetting agent, 2-5% of thickening agent, 2-4% of stabilizer and the balance of dispersion medium being 100%. The insecticidal effect is better under the condition of optimizing the proportion and the content of the effective components.
Preferably, the total content of tolfenpyrad and spirotetramat in the insecticidal composition is 20-40wt%, and under the content range of the effective components, the components between the tolfenpyrad and the spirotetramat and the auxiliary agent are more stable in the system and have better drug effect.
Experiments prove that the dispersible oil suspending agent provided by the invention has strong adhesive force, can better play the synergistic effect of active ingredients, greatly improves the insecticidal rate, can effectively prevent and kill piercing-sucking mouthpart pests, is convenient to use, can be used for not only conventional spraying, but also spraying of plant protection unmanned aerial vehicles, and has the advantages of difficult volatilization of liquid medicine, drift resistance, strong wetting and spreading property, good permeability and conductivity and rain wash resistance.
The invention also provides a preparation method of the dispersible oil suspending agent, which comprises the following steps:
(1) adding a dispersion medium, an emulsifier, a dispersant, a wetting agent and a stabilizer into a reaction kettle, and fully mixing and uniformly dispersing;
(2) adding the thickening agent, tolfenpyrad and spirotetramat into a reaction kettle under high-speed shearing, shearing for 10-35 minutes, and then grinding until the particle size D of the mixture is90Is less than 5 mu m, and the dispersible oil suspending agent of tolfenpyrad and spirotetramat is obtained.
Further, in the step (2), the materials are subjected to high-speed shearing at a shearing speed of 2500-.
Further, in the step (2), the grinding can be performed by any grinding method disclosed in the prior art, for example, the grinding can be performed under zirconia bead grinding media. After grinding, detecting by a laser particle size distribution instrument until the particle diameter D90Less than 5 mu m.
According to the invention, tolfenpyrad and spirotetramat are compounded to prepare the insecticidal composition, and the compounding of tolfenpyrad and spirotetramat effectively improves the insecticidal effect and enlarges the control range of insect pests. In addition, the tolfenpyrad and the spirotetramat are prepared into the dispersible oil suspending agent, the preparation can be suitable for dispersing and exerting tolfenpyrad and spirotetramat simultaneously, the drug effect is effectively improved, and compared with the preparation such as missible oil, powder, suspending agent and the like, the preparation has the advantages of strong dispersion stability, strong adhesiveness and permeability, convenience in use, no dust in the preparation process, more environment-friendly auxiliary agent and difficulty in causing pollution to the environment, human beings and livestock.
The insecticidal composition of tolfenpyrad and spirotetramat and the dispersible oil suspending agent thereof can be used for preventing and controlling insect pests in fruit and vegetable crop fields, wherein the fruit and vegetable can be cucumbers, hot peppers, tomatoes, oranges, pears and the like, and the insect pests are preferably piercing-sucking mouthparts pests, such as whiteflies, aphids, psyllids, plant hoppers, scale insects, thrips, red spiders and the like.
The invention has the following beneficial effects:
1. the tolfenpyrad and the spirotetramat are compounded, so that the tolfenpyrad and spirotetramat are widely applied to fruit and vegetable crops such as cucumbers, peppers, tomatoes, oranges, pears and the like, and can be used for preventing and controlling piercing-sucking mouthpart pests such as whiteflies, aphids, psyllids, plant hoppers, scale insects, thrips, red spiders and the like of the crops, and compared with a single agent of tolfenpyrad and spirotetramat, the insecticidal effect is obviously improved.
2. The invention prepares tolfenpyrad and spirotetramat into the dispersible oil suspending agent, greatly reduces the processing difficulty of the preparation formulation through the selection of the auxiliary agent, improves the stability of the preparation formulation, ensures that the finally obtained dispersible oil suspending agent has the advantages of good emulsifying dispersibility, difficult thickening or bottom forming, less residue after pouring, high suspension rate, good heat storage stability and the like, and effectively solves the problems of oil precipitation or caking, flocculation, particle size growth and the like in sample storage.
3. The dispersible oil suspending agent disclosed by the invention is simple in preparation process, easy to operate, convenient to use, not only can be used for conventional spraying, but also can be used for spraying of a plant protection unmanned aerial vehicle, the liquid medicine is not easy to volatilize, is resistant to drift, strong in wetting and spreading property, good in permeation conductivity, resistant to rain washing, high in target bioactivity, and strong in adhesion and permeability compared with dosage forms such as missible oil, powder and suspending agent, and the insecticidal effect on small piercing-sucking mouthpart pests is improved.
Detailed Description
The present invention is further illustrated by the following specific examples, which are intended to be merely exemplary and not limiting of the spirit of the invention.
The following percentages are by weight unless otherwise specified.
Example 115% Tolfenpyrad spirotetramat dispersible oil suspension
The formula is as follows: the effective components of tolfenpyrad 10%, spirotetramat 5%, emulsifier castor oil polyoxyethylene ether 2%, phenethyl phenol polyoxyethylene polyoxypropylene ether poly-3%, dispersant naphthalene sulfonic acid formaldehyde condensate sodium salt 2%, dioctyl sodium sulfosuccinate 1%, wetting agent sodium dodecyl sulfate 1%, thickener polyvinyl alcohol 2%, magnesium aluminum silicate 4%, stabilizer tributyl phosphate 2%, and the balance of dispersion medium palm oil.
The preparation method comprises the following steps: adding emulsifier into dispersion medium, dispersingAdding the agent, the wetting agent and the stabilizing agent into a reaction kettle with a shearing device, and fully mixing, emulsifying and uniformly dispersing; adding the thickening agent, tolfenpyrad and spirotetramat into the reaction kettle under the high-speed shearing state (2500-90And (5) obtaining 15% of tolfenpyrad-spirotetramat dispersible oil suspending agent until the particle size is less than 5 mu m.
Example 220% Tolfenpyrad-Spirotetramat dispersible oil suspension
The formula is as follows: the pesticide composition comprises the following effective components of 10% of tolfenpyrad, 10% of spirotetramat, 5% of alkylphenol formaldehyde resin polyoxyethylene ether serving as an emulsifier, 5% of sorbitan monostearate, 6.4% of calcium lignosulfonate serving as a dispersant, 1.6% of sodium dodecyl benzene sulfonate, 1.5% of succinic acid half ester sulfonate serving as a alkylphenol polyoxyethylene ether formaldehyde condensate serving as a wetting agent, 1.5% of nekal BX, 1% of fumed silica serving as a thickening agent, 1% of organic bentonite, 2% of butyl hydroxy anisole serving as a stabilizer and the balance of methyl oleate serving as a dispersion medium. The preparation method is the same as example 1.
Example 330% Tolfenpyrad spirotetramat dispersible oil suspension
The formula is as follows: the effective components of tolfenpyrad 20%, spirotetramat 10%, emulsifier alkylphenol formaldehyde resin polyoxyethylene ether 15%, sorbitan monostearate 5%, dispersant calcium lignosulfonate 4%, sodium dodecyl benzene sulfonate 2%, wetting agent alkylphenol polyoxyethylene ether formaldehyde condensate succinic acid half ester sulfonic acid sodium salt 1%, nekal BX 2%, thickener gas phase method silicon dioxide 2%, organic bentonite 3%, stabilizer butyl hydroxy anisole 3%, and the balance of dispersing medium methyl oleate. The preparation method is the same as example 1.
Example 440% Tolfenpyrad spirotetramat dispersible oil suspension
The formula is as follows: 30% of tolfenpyrad, 10% of spirotetramat, 10% of alkylphenol formaldehyde resin polyoxyethylene ether serving as an emulsifier, 5% of sorbitan monostearate, 2% of calcium lignosulfonate serving as a dispersant, 2% of sodium dodecyl benzene sulfonate, 1.5% of sodium succinate half-ester sulfonate serving as a alkylphenol polyoxyethylene formaldehyde condensate serving as a wetting agent, 4.5% of nekal BX, 0.5% of fumed silica serving as a thickener, 2% of organic bentonite, 3% of butyl hydroxy anisole serving as a stabilizer and the balance of methyl oleate serving as a dispersion medium. The preparation method is the same as example 1.
Example 540% Tolfenpyrad-Spirotetramat dispersible oil suspension
The formula is as follows: the effective components of tolfenpyrad 20%, spirotetramat 20%, emulsifier calcium dodecyl benzene sulfonate 5%, polyoxyethylene ether 10%, dispersant styrene-sodium methacrylate copolymer 1%, calcium lignosulfonate 1%, wetting agent nekal BX 2%, lauryl alcohol ether sodium sulfate 3%, thickener xanthan gum 0.7%, organic bentonite 0.3%, stabilizer sodium benzoate 1%, and the balance of dispersion medium epoxidized soybean oil. The preparation method is the same as example 1.
Example 645% Tolfenpyrad-spirotetramat dispersible oil suspension
The formula is as follows: the pesticide composition comprises 35% of tolfenpyrad, 10% of spirotetramat, 10% of alkylphenol polyoxyethylene ether serving as an emulsifier, 15% of sorbitan monostearate, 4% of a naphthalene sulfonic acid formaldehyde condensate sodium salt serving as a dispersant, 2% of dioctyl sodium sulfosuccinate, 3% of lauryl alcohol ether sodium sulfate serving as a wetting agent, 5% of lauryl sodium sulfate, 3% of magnesium aluminum silicate serving as a thickener, 2% of polyvinyl alcohol, 2% of triphenyl phosphite serving as a stabilizer and the balance of corn oil serving as a dispersion medium. The preparation method is the same as example 1.
Example 750% Tolfenpyrad spirotetramat dispersible oil suspension
The formula is as follows: the effective components of tolfenpyrad 40%, spirotetramat 10%, emulsifier alkylphenol formaldehyde resin polyoxyethylene ether 12%, sorbitan monostearate 6%, dispersant calcium lignosulfonate 2%, sodium dodecyl benzene sulfonate 1%, wetting agent alkylphenol polyoxyethylene ether formaldehyde condensation succinic acid half ester sulfonic acid sodium salt 2%, nekal BX 3%, thickener gas phase method silicon dioxide 1%, organic bentonite 3%, stabilizer butyl hydroxy anisole 4%, and the balance of dispersing medium methyl oleate. The preparation method is the same as example 1.
Example 835% Tolfenpyrad spirotetramat dispersible oil suspension
The formula is as follows: the effective components of tolfenpyrad 25%, spirotetramat 10%, emulsifier castor oil polyoxyethylene ether 12%, phenethyl phenol polyoxyethylene polyoxypropylene ether 5%, dispersant sodium dodecyl benzene sulfonate 6%, naphthalene sulfonic acid formaldehyde condensate sodium salt 4%, wetting agent nekal BX 5%, sodium dodecyl sulfonate 1%, thickener xanthan gum 2%, polyvinyl alcohol 2%, stabilizer triphenyl phosphite 5%, and the balance of dispersion medium castor oil. The preparation method is the same as example 1.
Comparative example 30% Tolfenpyrad-spirotetramat dispersible oil suspension
The formula is as follows: the effective components of tolfenpyrad 20%, spirotetramat 10%, emulsifier polysorbate 15%, calcium dodecyl benzene sulfonate 12%, dispersant ethylene oxide-propylene oxide block copolymer 0.5%, methylene dinaphthalene sodium sulfonate 0.3%, wetting agent fatty alcohol polyoxyethylene ether sodium sulfate 9%, thickener carboxymethyl cellulose 3%, diatomite 4%, stabilizer triphenyl phosphite 3%, and the balance of epoxidized soybean oil. The preparation method is the same as example 1.
The properties of the dispersible oil suspensions prepared in the above examples and comparative examples were measured, and the results are shown in table 1 below. Wherein, the suspension percentage is detected according to a method for measuring the suspension percentage of the pesticide GB/T14825-2006, the pourability is detected according to a method for measuring the pourability of the pesticide GB/T31737-2015, and the dispersion stability is detected according to CIPAC MT 180 measuring the dispersion stability of the suspoemulsion by the International Committee for pesticide analysis and collaboration. The heat storage stability is tested according to the method for testing the heat storage stability of the pesticide GB/T19136-2003.
Figure 441677DEST_PATH_IMAGE001
As can be seen from Table 1, the dispersible oil suspending agent obtained in the example of the invention meets the requirements in appearance, the suspension rate can reach more than 90%, the heat storage stability is good, the comparative example has poor quality before and after heat storage, the quality of the examples 1, 5, 6 and 8 is slightly poor after heat storage, and the quality of the examples 2-4 and 7 is good before and after heat storage, so that the preferable auxiliary agent plays a key role in the product quality. As can be seen from examples 2-4 and example 7, the properties of the resulting dispersible oil suspensions were similar when the preferred adjuvant was chosen, with varying amounts of the pharmaceutically active ingredient in the range of 20-50%, indicating that the drug content had less effect on the dosage form performance with the preferred adjuvant ingredients and amounts. It can be seen from examples 1, 5, 6, and 8 that in the case of the conventional adjuvant, the obtained dispersible oil suspension agent has relatively poor performance, and the replacement adjuvant has no significant effect improvement, which indicates that the components and content of the preferred adjuvant have significant improvement effect on the performance of the tolfenpyrad-spirotetramat dispersible oil suspension agent, and the conventional adjuvant does not.
Field test example 1: pesticide effect test for preventing and controlling tomato bemisia tabaci through field test
The test is carried out in vegetable base of Shouguang city, Shandong province, and the reference agents are 15% tolfenpyrad suspending agent and 22.4% spirotetramat suspending agent (purchased from market). The total number of 4 treatments are respectively as follows: treatment 1: spraying clear water, and blank control; and (3) treatment 2: the tolfenpyrad-spirotetramat dispersible oil suspending agent obtained in examples 1-8 and comparative example; and (3) treatment: 15% tolfenpyrad suspension concentrate; and (4) treatment: 22.4% spirotetramat suspension.
Wherein, the tolfenpyrad-spirotetramat dispersible oil suspending agent obtained in examples 1-8 and comparative example is subjected to stem and leaf spraying treatment according to the effective component dosage of 90 g/hectare, the treatment 3 is subjected to stem and leaf spraying treatment according to the effective component dosage of 112.5 g/hectare, and the treatment 4 is subjected to stem and leaf spraying treatment according to the effective component dosage of 100.8 g/hectare.
Bemisia tabaci was in the prime stage during the test. The pesticide is applied for 1 time by a worker-farm-16 knapsack manual sprayer, 750kg of water is added to prepare liquid medicine according to the dosage of the preparation per hectare, and the liquid medicine is uniformly sprayed according to the amount of the liquid medicine in the community. The weather during the test was good, and the daily average temperature was 21-30.0 ℃. No rain is present on the day of application, and no rain is present within 21 days after application.
Investigating population base before applying the pesticide, investigating live insect quantity in 3 rd, 14 th and 21 th days after the pesticide, calculating population decline rate, and observing the safety of the test medicament to crops.
The survey statistical method comprises the following steps: each survey of 15 crops identified in each plot, leaves were carefully examined on their backs without frightening the insects, and the number of live adults was recorded, and leaves were examined in the morning when the adults were less active.
Figure 787208DEST_PATH_IMAGE002
Figure 796621DEST_PATH_IMAGE003
As can be seen from the test results in the above table 2, the combination of tolfenpyrad and spirotetramat has a good control effect on tomato bemisia tabaci, and the population reduction rate is superior to that of tolfenpyrad suspending agents and spirotetramat suspending agents. As can be seen from the comparison of the drug effects of the examples and the comparative examples, the selection of the auxiliary agent has important influence on the play of the active ingredients, and improper selection of the auxiliary agent can seriously influence the compounding effect of the tolfenpyrad and the spirotetramat. According to the observation of the whole field test process, the tomatoes have good growth vigor within the test dose range, and the pesticide damage phenomenon does not occur in each treatment agent, which indicates that the tomatoes are safe.
Field test example 2: pesticide effect test for preventing and controlling pear psylla in field test
The test is arranged in a pear planting demonstration garden of Dangshan, Anhui, wherein the control agents are 15% of tolfenpyrad suspending agent and 22.4% of spirotetramat suspending agent (purchased from market). The total number of 4 treatments are respectively as follows: treatment 1: spraying clear water, and blank control; and (3) treatment 2: the tolfenpyrad-spirotetramat dispersible oil suspending agent obtained in examples 1-8 and comparative example; and (3) treatment: 15% tolfenpyrad suspension concentrate; and (4) treatment: 22.4% spirotetramat suspension. The test agents and dosages are shown in table 3.
The cultivation conditions and water and fertilizer management of each district are uniform and consistent. The pesticide is applied by a manual sprayer with the dosage of 3000kg/ha, and the front and back sides of the pear tree leaves in each district are required to be uniformly applied with pesticide. A blank control was also set, with 4 replicates per treatment, 5 trees per plot. Investigating population base before medicine, investigating live insect quantity in 3 rd, 14 th and 21 th days after medicine, calculating population decline rate, and observing safety of the test medicament to crops.
The survey statistical method comprises the following steps: 4 trees are investigated in each cell, 5 branches are fixed in each tree in 5 directions, the number of live insects on 20 leaves is randomly investigated in each branch, and if the number of insects is not less than 300 in each treatment, the number of the live insects is randomly investigated in each branch.
Figure 266917DEST_PATH_IMAGE002
Figure 121609DEST_PATH_IMAGE004
As can be seen from the test results in Table 3 above, the combination of tolfenpyrad and spirotetramat has a good control effect on psylla chinensis, and the population reduction rate is superior to that of tolfenpyrad suspending agents and spirotetramat suspending agents. As can be seen from the comparison of the drug effects of the examples and the comparative examples, the selection of the auxiliary agent has important influence on the play of the active ingredients, and improper selection of the auxiliary agent can seriously influence the compounding effect of the tolfenpyrad and the spirotetramat. According to the observation of the whole field test process, the pear trees grow well within the test dosage range, and the pesticide damage phenomenon does not occur in each treatment agent, which indicates that the pear trees are safe.
It should be understood that the above-described specific embodiments are merely illustrative of the present invention and are not intended to limit the present invention. Obvious variations or modifications which are within the spirit of the invention are possible within the scope of the invention.

Claims (9)

1. An insecticidal composition characterized by: the effective components are tolfenpyrad and spirotetramat, the content of tolfenpyrad in the insecticidal composition is 10-40wt%, the content of spirotetramat in the insecticidal composition is 5-25wt%, the dosage form is a dispersible oil suspending agent, and the dispersible oil suspending agent comprises the following effective components and auxiliary agents in percentage by weight: 10-40% of tolfenpyrad, 5-25% of spirotetramat, 5-25% of emulsifier, 2-10% of dispersant, 2-8% of wetting agent, 1-6% of thickening agent, 1-5% of stabilizing agent and the balance of dispersion medium being 100%;
the auxiliary agents of the dispersible oil suspending agent are an emulsifier, a dispersant, a wetting agent, a thickener, a stabilizer and a dispersion medium; the emulsifier is formed by mixing alkylphenol formaldehyde resin polyoxyethylene ether and sorbitan monostearate according to the mass ratio of 1-3: 1; the dispersing agent is formed by mixing calcium lignosulphonate and sodium dodecyl benzene sulfonate according to the mass ratio of 1-4: 1; the wetting agent is formed by mixing alkylphenol polyoxyethylene ether formaldehyde condensation product succinic acid half ester sulfonic acid sodium salt and nekal BX according to the mass ratio of 1: 1-3; the thickening agent is formed by mixing fumed silica and organic bentonite according to the mass ratio of 1: 1-4; the stabilizer is butyl hydroxy anisole; the dispersion medium is methyl oleate.
2. The insecticidal composition as claimed in claim 1, wherein: the total content of the effective components in the insecticidal composition is 15-50 wt%.
3. The insecticidal composition according to claim 1 or 2, characterized in that: the mass ratio of tolfenpyrad to spirotetramat is 1-4: 1.
4. The insecticidal composition according to claim 3, characterized in that: the mass ratio of tolfenpyrad to spirotetramat is 3: 1.
5. The insecticidal composition as claimed in claim 1, wherein: the composition consists of the following effective components and auxiliary agents in percentage by weight: 15-50% of active ingredients, 10-20% of emulsifier, 3-8% of dispersant, 3-6% of wetting agent, 2-5% of thickening agent, 2-4% of stabilizer and the balance of dispersion medium to 100%.
6. The insecticidal composition as claimed in claim 1, wherein: the composition consists of the following effective components and auxiliary agents in percentage by weight: 30% of tolfenpyrad, 10% of spirotetramat, 10-20% of emulsifier, 3-8% of dispersant, 3-6% of wetting agent, 2-5% of thickening agent, 2-4% of stabilizer and the balance of dispersion medium being 100%.
7. A process for the preparation of an insecticidal composition according to any one of claims 1 to 6, characterized in that it comprises the following steps:
(1) adding a dispersion medium, an emulsifier, a dispersant, a wetting agent and a stabilizer into a reaction kettle, and fully mixing and uniformly dispersing;
(2) adding the thickening agent, tolfenpyrad and spirotetramat into a reaction kettle under high-speed shearing, shearing for 10-35 minutes, and then grinding until the particle size D of the mixture is90Is less than 5 mu m, and the dispersible oil suspending agent of tolfenpyrad and spirotetramat is obtained.
8. Use of the insecticidal composition according to any one of claims 1 to 6 for controlling insect pests, characterized in that: the insect pests are sucking mouthparts pests in fruits and vegetables.
9. Use according to claim 8, characterized in that: the insect pest is whitefly, aphid, psylla, scale insect, thrips or red spider.
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