CN110200003B - Insecticidal composition of diafenthiuron and fenoxycarb and application thereof - Google Patents

Insecticidal composition of diafenthiuron and fenoxycarb and application thereof Download PDF

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CN110200003B
CN110200003B CN201910506428.6A CN201910506428A CN110200003B CN 110200003 B CN110200003 B CN 110200003B CN 201910506428 A CN201910506428 A CN 201910506428A CN 110200003 B CN110200003 B CN 110200003B
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diafenthiuron
fenoxycarb
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insecticidal composition
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CN110200003A (en
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袁良国
尹晓艺
段有春
张阔斌
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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
    • 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
    • A01N47/10Carbamic acid derivatives, i.e. containing the group —O—CO—N<; Thio analogues thereof
    • A01N47/12Carbamic acid derivatives, i.e. containing the group —O—CO—N<; Thio analogues thereof containing a —O—CO—N< group, or a thio analogue thereof, neither directly attached to a ring nor the nitrogen atom being a member of a heterocyclic ring
    • 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<
    • A01N47/30Derivatives containing the group >N—CO—N aryl or >N—CS—N—aryl

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  • General Health & Medical Sciences (AREA)
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  • Engineering & Computer Science (AREA)
  • Pest Control & Pesticides (AREA)
  • Agronomy & Crop Science (AREA)
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  • Environmental Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Dispersion Chemistry (AREA)
  • Toxicology (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)

Abstract

The invention discloses an insecticidal composition of diafenthiuron and fenoxycarb and application thereof, wherein the diafenthiuron and the fenoxycarb are compounded to have a good synergistic interaction effect, and the mass ratio of the diafenthiuron to the fenoxycarb is 1-10:1, preferably 1-5: 1. The insecticidal composition provided by the invention has the advantages that the insecticidal spectrum is expanded, the drug duration is improved, the generation of drug resistance is avoided, the insecticidal composition has a good effect on preventing and treating lepidoptera pests such as cotton bollworms, diamond back moths, stem borers, noctuids and the like in grain crops and vegetables, the sustainable development of the environment is facilitated, and the preparation process of the composition is environment-friendly and has no safety and pollution problems.

Description

Insecticidal composition of diafenthiuron and fenoxycarb and application thereof
Technical Field
The invention relates to an insecticidal composition, in particular to an insecticidal composition of diafenthiuron and fenoxycarb and application of the composition in controlling insect pests of grain crops and vegetables, and belongs to the technical field of pesticides.
Background
Diafenthiuron (Diafonthiuron) belongs to a novel thiourea insecticide, thiourea group on the molecular structure of the Diafenthiuron becomes a carbodiimide compound under the action of sunlight and multifunctional oxidase in insect bodies, the compound has extremely strong poisoning capacity on pest and pest mites, is a mitochondrial ATP enzyme inhibitor, and has the main action mechanism of interfering the energy metabolism of a nervous system, hindering ATP synthesis and damaging the basic functions of the nervous system. Diafenthiuron has systemic, contact, stomach toxicity and fumigation effects, and can be widely applied to field crops, fruit trees, vegetables and ornamental plants to control phytophagous mites and lepidoptera pests, such as diamondback moths, beet armyworms, whiteflies, aphids, leafhoppers and other pests.
Fenoxycarb (fenoxycarb) belongs to a non-terpene carbamate compound, has stomach toxicity and contact killing effects, has an insect growth regulation effect, is wide in insecticidal spectrum, has strong juvenile hormone activity on various insects, can kill eggs, inhibit metamorphosis of insects in an adult stage and molting of insects in a larval stage, causes death of the insects in a later stage or a pupal stage, is long in lasting period and difficult to generate resistance, and can be widely used for preventing and controlling sanitary pests, forest pests, storage pests and farmland pests.
Pesticide varieties containing a single active ingredient often have different degrees of defects in agricultural pest control, such as: the insecticidal spectrum is narrow, pests are easy to generate drug resistance after continuous use, the environmental pollution can be aggravated by using more times, and the defects can be effectively overcome by compounding active ingredients with different action mechanisms. Meanwhile, the synergistic effect generated by mixing the two active components can improve the control effect, expand the insecticidal spectrum, delay the generation of the drug resistance of pests and reduce the environmental pollution, thus being an important means for comprehensively controlling the pests. However, in most cases, the compounding effect of the pesticide is additive, and the compounding with synergistic effect is less, especially the compounding with very obvious synergistic effect and very high co-toxicity coefficient is less. At present, the combination of the two active ingredients of diafenthiuron and fenoxycarb is not reported.
Disclosure of Invention
The invention aims to provide an insecticidal composition of diafenthiuron and fenoxycarb, wherein the active pharmaceutical ingredients of the insecticidal composition are diafenthiuron and fenoxycarb which are compounded according to a specific proportion, the action mechanisms of the diafenthiuron and the fenoxycarb are different, and the good synergistic effect is generated by verifying the compounding of the diafenthiuron and the fenoxycarb, so that the insecticidal spectrum is expanded, the generation of drug resistance is slowed down, the insecticidal effect is improved, and the sustainable development of the environment is facilitated.
The invention also provides the application of the insecticidal composition in controlling the insect pests of grain crops and vegetables, the preparation process of the insecticidal composition is environment-friendly and safe, the pollution problem is avoided, the insecticidal spectrum is wide, the insecticidal effect is good, and the insecticidal composition has better use experience compared with a single medicinal active ingredient preparation.
Through research and a large number of indoor and field tests, the inventor finds that the compound of diafenthiuron and fenoxycarb can generate good synergistic action, and obtains the insecticidal composition. The specific technical scheme of the invention is as follows:
the insecticidal composition takes the diafenthiuron and the fenoxycarb as active pharmaceutical ingredients, and the mass ratio of the diafenthiuron to the fenoxycarb is 1-10:1, preferably 1-5: 1.
Furthermore, the insecticidal composition comprises an auxiliary agent besides the pharmaceutical active ingredient, and the content of the pharmaceutical active ingredient in the insecticidal composition is 20-60 wt%.
Furthermore, the insecticidal composition can be prepared into any feasible agriculturally acceptable dosage forms according to the methods known by the person skilled in the art, such as suspending agents, and when the composition is prepared into different dosage forms, the auxiliary agents are different. Wherein, the research and the selection of the auxiliary agent can improve the performance and the using effect of each preparation.
In the insecticidal composition, the diafenthiuron technical is white crystal, has higher solubility in organic solvent and a melting point of 144.6-147.7 ℃, and is usually processed into missible oil, wettable powder, suspending agent and other formulations in production; fenoxycarb is colorless crystal, has high solubility in organic solvent, has a melting point of 53-54 ℃ (lower than 60 ℃), and is often processed into missible oil and wettable powder in production and into suspending agents with certain difficulty (the melting point is lower). Therefore, the diafenthiuron and fenoxycarb are difficult to prepare into the aqueous suspension, and the auxiliary agent needs to be screened and tested, so that the aqueous suspension is suitable for the diafenthiuron and the fenoxycarb.
Furthermore, the invention researches and screens the auxiliary agent of the suspending agent aiming at the characteristics of the active ingredients of the medicine, and obtains a preferable suspending agent formulation by selecting and matching the wetting agent and the dispersing agent. The suspending agent consists of the following pharmaceutical active ingredients and auxiliary agents in percentage by weight: 20-60% of active ingredients of the medicine, 1-10% of dispersing agent, 2-15% of wetting agent, 0.1-1% of thickening agent, 0.5-3% of defoaming agent, 1-5% of antifreezing agent and water for supplementing 100%. Wherein, the dispersing agent, the wetting agent, the thickening agent, the defoaming agent, the antifreezing agent and the water are collectively called as the auxiliary agent.
Preferably, the suspending agent consists of the following pharmaceutical active ingredients and auxiliary agents in percentage by weight: 20-60% of active pharmaceutical ingredients (preferably 30-50%), 4-6% of dispersing agent, 3-8% of wetting agent, 0.5% of thickening agent, 1% of defoaming agent, 2% of antifreezing agent and water to make up 100%.
Further, in the suspending agent, the dispersing agent is one or more of calcium lignosulfonate, sodium alkyl naphthol sulfonic acid formaldehyde condensate, nonylphenol polyoxyethylene ether, acrylic acid-maleic anhydride copolymer, ethylene oxide-propylene oxide block copolymer and sodium dodecyl benzene sulfonate, and is preferably formed by mixing acrylic acid-maleic anhydride copolymer and nonylphenol polyoxyethylene ether according to the weight ratio of 1-3: 1.
Further, in the suspending agent, the wetting agent is one or more of sodium tetradecyl sulfate, alpha-olefin sulfonate, alkylphenol polyoxyethylene succinic acid half ester sulfonate sodium salt, alkyl succinate sulfonate, alkyl naphthalene sodium sulfonate, sodium lignin sulfonate and sodium ethyl laurate sulfonate, and is preferably formed by mixing alkyl naphthalene sodium sulfonate and sodium ethyl laurate sulfonate according to a weight ratio of 1: 1-4.
Further, in the above suspending agent, the thickener is one or more of gum arabic, polyvinyl alcohol, organobentonite, xanthan gum and magnesium aluminum silicate, and xanthan gum is preferred.
Further, in the defoaming agent, the defoaming agent is silicone oil or C10-20Saturated fatty acid compound, C8-10One or more of fatty alcohol compounds, preferably silicone oil.
Further, in the above suspending agent, the anti-freezing agent is one or more of ethylene glycol, propylene glycol and glycerol, and is preferably ethylene glycol.
The invention also provides a preparation method of the preferable suspending agent, which comprises the following steps:
(1) shearing water, a dispersing agent, a wetting agent and a defoaming agent at a high speed, and uniformly mixing;
(2) adding the medicinal active ingredients diafenthiuron and fenoxycarb into the mixture obtained in the step (1), and sanding the mixture by using a sand mill until the particle size of the product is below 5 mu m;
(3) and (3) adding the thickening agent into the antifreezing agent, uniformly mixing, adding the thickening agent into the liquid mixture after sanding in the step (2), and carrying out high-speed shearing and uniform mixing to obtain the suspending agent of the insecticidal composition.
The composition is mainly used for controlling insect pests in food crops and vegetables, and the insect pests are preferably lepidoptera pests, such as cotton bollworms, plutella xylostella, stem borers, noctuids and the like.
The invention has the beneficial effects that:
1. the active ingredients of the insecticidal composition provided by the invention are diafenthiuron and fenoxycarb, which belong to two insecticides with different action mechanisms, and the diafenthiuron and the fenoxycarb are mixed with each other without conflict, so that the insecticidal spectrum is expanded, and the insecticidal efficiency is improved.
2. The insecticidal composition has good synergistic effect in a certain mass ratio range, the control effect is higher than that of a single agent, the dosage is small, the generation of insect pest resistance to drugs is delayed, and the environmental sustainable development is facilitated;
3. the insecticidal composition has special effect on the lepidoptera pests such as cotton bollworms, plutella xylostella, borers, noctuids and the like on grain crops and vegetables, and has good application prospect.
4. According to the invention, the diafenthiuron and the fenoxycarb are prepared into the suspending agent, and the obtained suspending agent has excellent performance, low foamability, high suspension rate, less residue after pouring, good heat storage stability and improved insecticidal control effect.
Detailed Description
The following specific examples are given to illustrate the technical aspects of the present invention in detail, but the present invention is not limited to these examples. Unless otherwise specified, the following components are contained in weight percent.
The embodiment of the invention adopts a method combining indoor toxicity measurement and field test. Firstly, indoor toxicity measurement is carried out according to the Sun Yunpei method, the cotoxicity coefficient (CTC) of the two medicaments compounded according to a certain proportion is determined, the CTC is less than 80 and is antagonistic, the CTC is more than or equal to 80 and is less than or equal to 120 and is additive, and the CTC is more than 120 and is synergistic, and then field efficacy test is carried out on the basis.
And (3) measuring the indoor toxicity of the diafenthiuron and fenoxycarb compound to cabbage diamondback moth larvae.
The test agents were provided by Shandong Weifang Runfeng Feng chemical company Limited.
And (3) experimental design: after the effective inhibition concentration range of each medicament is determined through pre-test, each medicament is respectively treated with a series of concentrations according to the content of effective components, and clear water is used for comparison. The method is carried out according to the standard pesticide for indoor bioassay of pesticides, the lethal medium concentration of the pesticide and the mixed pesticide is measured by a leaf soaking method, and the cotoxicity coefficient is obtained by a method for calculating the combined toxicity provided by Sun Yunpei et al (1960).
The calculation formula is as follows (using diafenthiuron as a standard medicament and the toxicity index is 100)
Figure 931454DEST_PATH_IMAGE001
The test results are shown in table 1:
Figure 379753DEST_PATH_IMAGE002
as can be seen from Table 1, diafenthiuron and fenoxycarb are effective in inhibiting the growth of larvae of Plutella xylostella5056.17mg/L and 78.35mg/L, respectively. The mass ratio of the diafenthiuron to the fenoxycarb is preferably 1-10:1, more preferably 1-5:1, and the mass ratio of the diafenthiuron to the fenoxycarb is preferably 1-10:1, more preferably 1-5:1, because the co-toxicity coefficients of the diafenthiuron to the fenoxycarb are respectively 138.53, 149.44, 137.84, 130.13 and 130.37 which are respectively greater than 120, and the synergistic effect is shown, and no synergistic effect is obtained when the mass ratio exceeds 10: 1.
After determining the mass ratio of the pharmaceutically active ingredients, they are formulated into suspensions with suitable adjuvants, and a few representative examples of suspensions are specifically, but not exclusively, listed below.
Example 120% diafenthiuron fenoxycarb suspension
The formula is as follows: the pharmaceutical active ingredients comprise 10 percent of diafenthiuron, 10 percent of fenoxycarb, 2 percent of dispersing agent acrylic acid-maleic anhydride copolymer, 2 percent of nonylphenol polyoxyethylene ether, 1 percent of wetting agent alkyl naphthalene sodium sulfonate, 2 percent of lauric acid ethyl ester sodium sulfonate, 0.5 percent of thickening agent xanthan gum, 1 percent of defoaming agent silicone oil, 2 percent of antifreezing agent ethylene glycol and 100 percent of water.
The preparation method comprises the following steps: shearing the dispersing agent, the wetting agent, the defoaming agent and water in the formula at a high speed, uniformly mixing, adding diafenthiuron and fenoxycarb, and sanding in a sand mill, wherein the grain size of the material needs to be frequently detected during sanding, and the grain size is sanded to be 3-5 mu m; adding the thickening agent into the antifreezing agent, uniformly mixing, then adding the mixture of the thickening agent and the antifreezing agent into the liquid mixture after sanding, and uniformly mixing by high-speed shearing to obtain the 20% diafenthiuron fenoxycarb suspending agent product.
Example 230% diafenthiuron fenoxycarb suspension
The formula is as follows: 20% of diafenthiuron serving as a medicinal active component, 10% of fenoxycarb, 3% of acrylic acid-maleic anhydride copolymer serving as a dispersing agent, 1% of nonylphenol polyoxyethylene ether, 2% of sodium alkylnaphthalene sulfonate serving as a wetting agent, 2% of sodium ethyl laurate sulfonate, 0.5% of xanthan gum serving as a thickening agent, 1% of silicone oil serving as a defoaming agent, 2% of ethylene glycol serving as an antifreezing agent and the balance of water to 100%. The preparation method is the same as example 1.
Example 340% diafenthiuron fenoxycarb suspension
The formula is as follows: 30% of diafenthiuron serving as a medicinal active component, 10% of fenoxycarb, 3% of acrylic acid-maleic anhydride copolymer serving as a dispersing agent, 1% of nonylphenol polyoxyethylene ether, 1% of sodium alkylnaphthalene sulfonate serving as a wetting agent, 4% of sodium ethyl laurate sulfonate, 0.5% of xanthan gum serving as a thickening agent, 1% of silicone oil serving as a defoaming agent, 2% of ethylene glycol serving as an antifreezing agent and the balance of water to 100%. The preparation method is the same as example 1.
Example 442% diafenthiuron fenoxycarb suspension
The formula is as follows: 35 percent of diafenthiuron serving as a medicinal active component, 7 percent of fenoxycarb, 2.5 percent of acrylic acid-maleic anhydride copolymer serving as a dispersing agent, 1.5 percent of nonylphenol polyoxyethylene ether, 0.6 percent of alkyl naphthalene sodium sulfonate serving as a wetting agent, 2.4 percent of ethyl laurate sodium sulfonate, 0.5 percent of xanthan gum serving as a thickening agent, 1 percent of silicon oil serving as a defoaming agent, 2 percent of ethylene glycol serving as an antifreezing agent and the balance of water accounting for 100 percent. The preparation method is the same as example 1.
Example 545% diafenthiuron fenoxycarb suspension
The formula is as follows: 40% of diafenthiuron serving as a medicinal active component, 5% of fenoxycarb, 3% of acrylic acid-maleic anhydride copolymer serving as a dispersing agent, 2% of nonylphenol polyoxyethylene ether, 1% of sodium alkylnaphthalene sulfonate serving as a wetting agent, 3% of sodium ethyl laurate sulfonate, 0.5% of xanthan gum serving as a thickening agent, 1% of silicone oil serving as a defoaming agent, 2% of ethylene glycol serving as an antifreezing agent and the balance of water to 100%. The preparation method is the same as example 1.
Example 650% diafenthiuron fenoxycarb suspension
The formula is as follows: the active pharmaceutical ingredients are 40 percent of diafenthiuron and phenoxy10% of carbofuran, 4% of calcium lignosulfonate dispersant, 2% of sodium alkyl naphthol sulfonate formaldehyde condensate, 1% of sodium tetradecyl sulfate wetting agent, 1% of sodium lignosulfonate, 0.5% of xanthan gum thickener and C defoaming agent10-200.5 percent of saturated fatty acid compounds, 1 percent of antifreeze propylene glycol and the balance of water to 100 percent. The preparation method is the same as example 1.
Example 755% diafenthiuron fenoxycarb suspension
The formula is as follows: 50% of diafenthiuron serving as a medicinal active component, 5% of fenoxycarb, 3% of acrylic acid-maleic anhydride copolymer serving as a dispersing agent, 3% of nonylphenol polyoxyethylene ether, 3% of sodium alkylnaphthalene sulfonate serving as a wetting agent, 4% of sodium ethyl laurate sulfonate, 0.5% of xanthan gum serving as a thickening agent, 1% of silicone oil serving as a defoaming agent, 2% of ethylene glycol serving as an antifreezing agent and the balance of water to 100%. The preparation method is the same as example 1.
Example 860% diafenthiuron fenoxycarb suspension
The formula is as follows: 45 percent of diafenthiuron serving as a medicinal active component, 15 percent of fenoxycarb, 2 percent of sodium dodecyl benzene sulfonate serving as a dispersant, 8 percent of ethylene oxide-propylene oxide block copolymer, 12 percent of wetting agent alpha-olefin sodium sulfonate, 3 percent of alkylphenol polyoxyethylene succinic acid half ester sulfonic acid sodium salt, 0.1 percent of polyvinyl alcohol serving as a thickening agent, and 0.1 percent of defoaming agent C8-101.5 percent of fatty alcohol compound, 2.5 percent of antifreeze glycerol and water which are complemented to 100 percent. The preparation method is the same as example 1.
Example 935% diafenthiuron fenoxycarb suspension
The formula is as follows: 30% of diafenthiuron serving as a medicinal active component, 5% of fenoxycarb, 2% of calcium lignosulfonate serving as a dispersant, 3% of sodium alkyl naphthol sulfonate formaldehyde condensate, 3% of alkyl succinate sulfonate serving as a wetting agent, 3% of sodium alkyl naphthalene sulfonate, 0.6% of magnesium aluminum silicate serving as a thickening agent, 3% of silicone oil serving as a defoaming agent, 4% of ethylene glycol serving as an antifreezing agent and the balance of water to 100%. The preparation method is the same as example 1.
Example 1040% diafenthiuron fenoxycarb suspension
The formula is as follows: 35 percent of diafenthiuron serving as a medicinal active component, 5 percent of fenoxycarb, 1.5 percent of acrylic acid-maleic anhydride copolymer serving as a dispersant, 4 percent of calcium lignosulfonate, 5 percent of sodium lignosulfonate serving as a wetting agent, 3 percent of alpha-olefin sulfonate, 0.7 percent of xanthan gum serving as a thickening agent, 0.5 percent of silicone oil serving as a defoaming agent, 5 percent of ethylene glycol serving as an antifreezing agent and the balance of water to 100 percent. The preparation method is the same as example 1.
Example 1160% diafenthiuron fenoxycarb suspension
The formula is as follows: 45% of diafenthiuron serving as a medicinal active component, 15% of fenoxycarb, 3% of acrylic acid-maleic anhydride copolymer serving as a dispersing agent, 2% of nonylphenol polyoxyethylene ether, 4% of sodium alkylnaphthalene sulfonate serving as a wetting agent, 4% of sodium ethyl laurate sulfonate, 0.5% of xanthan gum serving as a thickening agent, 1% of silicone oil serving as a defoaming agent, 2% of ethylene glycol serving as an antifreezing agent and the balance of water to 100%. The preparation method is the same as example 1.
Example 1230% diafenthiuron fenoxycarb suspension
The formula is as follows: 20 percent of diafenthiuron serving as a medicinal active component, 10 percent of fenoxycarb, 0.5 percent of dispersant ethylene oxide-propylene oxide block copolymer, 0.5 percent of calcium lignosulfonate, 1 percent of wetting agent tetradecyl sodium sulfate, 2 percent of alkyl succinate sulfonate, 1 percent of thickening agent organic bentonite and defoaming agent C10-201% of saturated fatty acid compounds, 2% of antifreeze propylene glycol and water to make up to 100%. The preparation method is the same as example 1.
Comparative example
The formula is as follows: 45 percent of diafenthiuron serving as a medicinal active component, 15 percent of fenoxycarb, 3 percent of phenethylnaphthol polyoxyethylene ether serving as a dispersant, 2 percent of styrene-sodium methacrylate copolymer, 8 percent of sorbitol stearate serving as a wetting agent, 0.5 percent of xanthan gum serving as a thickening agent, 1 percent of organic siloxane serving as a defoaming agent, 2 percent of sorbitol serving as an antifreeze and 100 percent of water. The preparation method is the same as example 1.
The properties of the products obtained in the above examples and comparative examples were measured and the results are shown in Table 2 below. The suspension rate is detected according to a GB/T14825-2006 pesticide suspension rate measuring method, the pourability is detected according to a GB/T31737-2015 pesticide pourability measuring method, and the lasting foamability is specified according to HG/T2467.5-2003 pesticide suspension agent product standard writing specifications: 4.11 the determination method of the long-lasting foamability test is used for detection, and the heat storage stability is determined according to the determination method of the heat storage stability of the GB/T19136-2003 pesticide.
Figure 690648DEST_PATH_IMAGE003
As can be seen from Table 2, compared with the examples, the comparative examples have poorer suspension rate, foamability and thermal stability, which shows that the selection of the auxiliary agent has important influence on the performance of the suspending agent, and the invention improves the performance of the suspending agent by screening the auxiliary agent and the content. The suspending agents of examples 6, 8, 9, 10, 12 had slightly poorer quality after hot storage, while the suspending agents of examples 1, 2, 3, 4, 5, 7, 11 using the preferred adjuvants had good quality both before and after hot storage, indicating that the selection of the preferred adjuvants improved the performance of the suspending agents.
Furthermore, it can be seen from examples 1 to 5 and examples 7 and 11 that, in the case of the selection of preferred adjuvants, the properties of the resulting suspensions were similar when the content of the pharmaceutically active ingredient was varied within the range of 20 to 60%, which means that with the preferred adjuvant ingredients and contents, the effect of the drug content on the properties of the dosage forms was less. It can be seen from examples 6, 8, 9, 10 and 12 that the performance of the resulting suspension concentrate is relatively poor with the use of conventional adjuvants, and there is no significant improvement in replacement adjuvants, indicating that the ingredients and levels of the preferred adjuvants have a significant effect on the performance of the diafenthiuron fenoxycarb suspension concentrate, whereas conventional adjuvants do not.
Test determination of compound field pesticide effect of diafenthiuron and fenoxycarb
1. Prevention and control of rice stem borer by field test
The pesticide effect test is carried out on the diafenthiuron and fenoxycarb suspending agents prepared in the above examples and comparative examples for preventing and treating the rice stem borer. The experiment is arranged to be carried out in the area of Changde city, Hunan province, and the contrast agents are 50% diafenthiuron suspending agent (purchased from the market) and 250g/L fenoxycarb suspending agent (purchased from the market).
The positive rice stem borers are in the initial stage when the pesticide is applied. And selecting 16 rice fields for testing, wherein one rice field is selected as a blank control area, the control area is clear water spray and is not sprayed with the pesticide, and the other rice fields are pesticide treatment areas and are sprayed with different suspending agents. The application method comprises the following steps: spraying 1 time with industrial and agricultural-16 knapsack hand sprayer, adding 450kg of suspending agent per hectare, and spraying uniformly. The weather during the test was good, and the daily average temperature was 22-30.0 ℃. No rain is present on the day of application, and no rain is present 14 days after application.
Investigating population base before applying pesticide, investigating live insect quantity in 3 rd, 7 th and 14 th days after pesticide application, calculating, correcting and preventing effect, and observing the safety of the test pesticide on crops.
The drug effect calculation method comprises the following steps:
Figure 617016DEST_PATH_IMAGE004
the control results of rice stem borer are shown in the following table 3:
Figure 198432DEST_PATH_IMAGE006
the test results in the table 3 show that the diafenthiuron and fenoxycarb can effectively prevent and control the rice stem borers after being compounded, the control effect on the rice stem borers 3 days, 7 days and 14 days after the pesticide application is obviously better than that of 2 control pesticides, and the synergistic effect is shown. The control effect of the examples 1-5, 7 and 11 using the preferred auxiliary agents and the preferred proportion is obviously better than that of other examples. According to the observation of the whole field test process, the rice grows well within the test dose range, and the pesticide damage phenomenon does not occur in each treatment agent, which indicates that the rice is safe to the rice.
And field experiment for preventing cabbage beet armyworm
The test is carried out in Shandong Shouguang vegetable base, and the initial stage of the beet armyworm generation is positive when the drug is applied. And selecting 16 cabbage growing areas for testing, wherein one cabbage growing area is selected as a blank control area, the control area is clear water spray without spraying a medicament, and the other testing areas are medicament treatment areas and are sprayed with different suspending agents. The application method comprises the following steps: spraying 1 time with industrial and agricultural-16 knapsack hand sprayer, adding 450kg of suspending agent per hectare, and spraying uniformly. The weather during the test was good, and the daily average temperature was 24-30.0 ℃. No rain is produced on the day of application, and no rain is produced 15 days after application.
Investigating population base before applying pesticide, investigating live insect quantity in 3 rd, 7 th and 14 th days after pesticide application, calculating, correcting and preventing effect, and observing the safety of the test pesticide on crops.
The drug effect calculation method comprises the following steps:
Figure 552053DEST_PATH_IMAGE007
the control results for cabbage loopers are shown in table 4 below:
Figure 350245DEST_PATH_IMAGE008
as can be seen from the test results in the table 4 above, the diafenthiuron and fenoxycarb can effectively prevent and control cabbage beet armyworms after being compounded, the control effect on the cabbage beet armyworms in 3 days, 7 days and 14 days after the pesticide application is obviously superior to that of 2 control agents, and the synergistic effect is shown. The control effect of the examples 1-5, 7 and 11 using the preferred auxiliary agents and the preferred proportion is obviously better than that of other examples. According to the observation of the whole field test process, the cabbage grows well within the test dose range, and the phenomenon of phytotoxicity does not occur in each treatment agent, which indicates that the cabbage is safe to the cabbage.

Claims (6)

1. An insecticidal composition characterized by: the diafenthiuron and fenoxycarb are used as active pharmaceutical ingredients, the mass ratio of the diafenthiuron to the fenoxycarb is 1-10:1, the dosage form of the diafenthiuron suspension is a suspending agent, and the suspending agent comprises the following components in percentage by weight: 20-60% of active ingredients of the medicine, 1-10% of dispersing agent, 2-15% of wetting agent, 0.1-1% of thickening agent, 0.5-3% of defoaming agent, 1-5% of antifreezing agent and the balance of water to 100%;
the dispersing agent is formed by mixing acrylic acid-maleic anhydride copolymer and nonylphenol polyoxyethylene ether according to the weight ratio of 1-3: 1; the wetting agent is formed by mixing sodium alkyl naphthalene sulfonate and sodium ethyl laurate sulfonate according to the weight ratio of 1: 1-4; the thickening agent is xanthan gum; the defoaming agent is silicone oil; the antifreezing agent is ethylene glycol.
2. The insecticidal composition as claimed in claim 1, wherein: the mass ratio of the diafenthiuron to the fenoxycarb is 1-5: 1.
3. The insecticidal composition as claimed in claim 1, wherein: the suspending agent consists of the following components in percentage by weight: 30-50% of active ingredients of the medicine, 4-6% of dispersing agent, 3-8% of wetting agent, 0.5% of thickening agent, 1% of defoaming agent, 2% of antifreezing agent and the balance of water to 100%.
4. Use of the insecticidal composition according to any one of claims 1 to 3 for controlling pests on food crops and vegetables.
5. Use according to claim 4, characterized in that: the insect pest is Lepidoptera pest.
6. Use according to claim 4, characterized in that: the insect pest is cotton bollworm, diamondback moth, stem borer or noctuid.
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CN102047897A (en) * 2009-10-29 2011-05-11 青岛海利尔药业有限公司 Pesticidal composition containing diafenthiuron
CN105152998A (en) * 2015-08-25 2015-12-16 海利尔药业集团股份有限公司 Methylthio-diafenthiuron pesticide and application thereof
CN107249330A (en) * 2015-05-06 2017-10-13 龙灯农业化工国际有限公司 Composition pesticide containing Methomyl and lufenuron

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CN1325627A (en) * 2001-07-11 2001-12-12 深圳市诺普信农化有限公司 Hexaflumuron carbosulfan insecticide composition
CN102047897A (en) * 2009-10-29 2011-05-11 青岛海利尔药业有限公司 Pesticidal composition containing diafenthiuron
CN107249330A (en) * 2015-05-06 2017-10-13 龙灯农业化工国际有限公司 Composition pesticide containing Methomyl and lufenuron
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