CN111053085A - Emamectin benzoate B2a and indoxacarb suspoemulsion and preparation method thereof - Google Patents
Emamectin benzoate B2a and indoxacarb suspoemulsion and preparation method thereof Download PDFInfo
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION 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
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/90—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having two or more relevant hetero rings, condensed among themselves or with a common carbocyclic ring system
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION 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
- A01N25/00—Biocides, 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
- A01N25/02—Biocides, 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
- A01N25/04—Dispersions, emulsions, suspoemulsions, suspension concentrates or gels
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION 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
- A01N47/00—Biocides, 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
- A01N47/08—Biocides, 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
- A01N47/28—Ureas or thioureas containing the groups >N—CO—N< or >N—CS—N<
- A01N47/38—Ureas or thioureas containing the groups >N—CO—N< or >N—CS—N< containing the group >N—CO—N< where at least one nitrogen atom is part of a heterocyclic ring; Thio analogues thereof
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Abstract
The invention relates to the technical field of pesticides, and particularly discloses a methylamino abamectin B2a benzoate and indoxacarb suspoemulsion and a preparation method thereof. The suspoemulsion comprises the following components in percentage by mass: 0.1-10% of methylamino abamectin B2a benzoate; 0.1-20% of indoxacarb; 2-5% of an emulsifier; 0.5-4% of a wetting agent; 1-8% of a dispersant; 0.1 to 1 percent of thickening agent; 0.3 to 0.7 percent of antifreeze; 0.1 to 0.3 percent of defoaming agent; 0.01-0.1% of a stabilizer; 0.1 to 2 percent of synergist; the balance being water. The suspoemulsion provided by the invention takes water as a solvent, is green and environment-friendly, has low cost, excellent quick action and persistence, can effectively reduce the pesticide application times and improve the medicament utilization rate, and has the disease prevention effect while killing pests, thereby having the effects of reducing the pesticide application synergistic effect and preventing multiple pesticides by one spraying.
Description
Technical Field
The invention relates to the technical field of pesticides, and particularly relates to an emamectin benzoate B2a benzoate and indoxacarb suspoemulsion and a preparation method thereof.
Background
The emamectin benzoate is a macrocyclic lactone pesticide prepared by biological fermentation, and has the characteristics of super-high efficiency, low toxicity, no residue, no public nuisance and the like. The emamectin benzoate has extremely high activity and strong quick action on larvae of lepidoptera insects (such as rice stem borers) and other pests and mites, but has short duration, and is time-consuming, labor-consuming and poor in effect when used alone.
Indoxacarb is a novel oxadiazine pesticide, has the effects of contact poisoning and stomach poisoning, enters the body of pests through contact and feeding, blocks sodium ion channels of the nervous systems of the pests, leads the pests to be paralyzed rapidly, and stops feeding. According to the insecticidal principle, the indoxacarb has poor quick-acting property and long lasting period, and when the indoxacarb is used alone, the death time of pests lasts long from the time of finding the pests to the time of applying the indoxacarb to the pests, so that the pests of crops are easy to suffer, and the yield is reduced.
The mixing of different pesticide varieties is a common method for preventing and controlling agricultural resistant pests, can effectively improve the actual prevention and control effect, and delays the generation of the drug resistance of the pests. Although the problems can be basically solved after the emamectin benzoate and the indoxacarb are mixed for use, more problems still exist in the preparation process, for example, when the emamectin benzoate and the indoxacarb are prepared into missible oil, the solvent amount and the auxiliary agent amount are too large, and the environment is easily polluted; when the oil suspending agent is prepared, a large amount of solvent and auxiliary agent are needed, and the solvent is mostly grease, so the cost is high; when the emamectin benzoate water suspension agent is prepared, the solubility of the emamectin benzoate in water is obvious along with the temperature change, the stability is poor, the emamectin benzoate water suspension agent is easy to agglomerate and is not easy to disperse during use, and the drug effect is influenced. Therefore, the development of an emamectin benzoate and indoxacarb preparation which has low cost, good drug effect, high stability and environmental protection is urgently needed.
Disclosure of Invention
Aiming at the technical problems in the prior art, the invention provides a methylamino abamectin B2a benzoate and indoxacarb suspoemulsion and a preparation method thereof.
In order to achieve the purpose of the invention, the embodiment of the invention adopts the following technical scheme:
the suspending emulsion of emamectin benzoate B2a and indoxacarb comprises the following components in percentage by mass: 0.1-10% of methylamino abamectin B2a benzoate; 0.1-20% of indoxacarb; 2-5% of an emulsifier; 0.5-4% of a wetting agent; 1-8% of a dispersant; 0.1 to 1 percent of thickening agent; 0.3 to 0.7 percent of antifreeze; 0.1 to 0.3 percent of defoaming agent; 0.01-0.1% of a stabilizer; 0.1 to 2 percent of synergist; the balance being water.
Compared with the prior art, the methylamino abamectin B2a benzoate and indoxacarb suspoemulsion provided by the invention takes water as a solvent, is green and environment-friendly, has low cost, adopts the combined action of a wetting agent, a dispersing agent, a defoaming agent, an emulsifying agent and a synergist and a plurality of assistants to improve the wettability and the dispersibility of a system, forms stable suspoemulsion, and has good permeability; meanwhile, the stability of the suspoemulsion is further improved by adding a thickening agent, an antifreezing agent and a stabilizing agent. The suspoemulsion has excellent quick-acting property and lasting property, can effectively reduce the application frequency and improve the utilization rate of the medicament, has the disease prevention effect while killing insects, and has the effects of reducing the application synergistic effect and preventing multiple diseases by one spray.
Further, the mass ratio of the emamectin benzoate B2a to the indoxacarb is 3:5-15, and the quick-acting property and the lasting property of the suspoemulsion are ensured through compounding of the emamectin benzoate B2a and the indoxacarb.
Furthermore, the wetting agent is an alkyl naphthalene sulfonate wetting agent, such as a mixture of alkyl naphthalene sulfonate and an anionic wetting agent, the active ingredient is greater than 95%, the wetting performance of the system is improved, meanwhile, the permeability of the suspoemulsion is improved, and the quick-acting performance of the suspoemulsion is improved.
Furthermore, the dispersing agent is an alkyl naphthalene sulfonate formaldehyde condensate, and the dispersing agent and a wetting agent act together to improve the wettability of the system, increase the dispersion degree of the medicine, further improve the permeability of the suspending agent and effectively improve the drug effect.
Furthermore, the emulsifier is isopropyl alkyl benzene sulfonate, has certain non-ionic property, and two hydrophobic methyl groups are arranged on a cationic group, so that the emamectin benzoate B2a and the indoxacarb can form a more stable suspension system in water, and simultaneously. The suspending agent and the wetting agent and the dispersing agent act together, so that the suspending agent has good wetting power and spreading performance, and is beneficial to improving the quick action of the suspending agent.
Furthermore, the defoaming agent is a silicone defoaming agent, can greatly reduce the surface tension of the suspoemulsion, and can be used together with other auxiliary agents to ensure that the suspoemulsion has more excellent wetting performance, can easily wet almost all kinds of leaf surfaces, and enhances the rain wash resistance and the penetration resistance of the suspoemulsion. Promote the quick absorption of the liquid medicine and provide the effective utilization rate of the pesticide.
Furthermore, the synergist is isooctanol polyoxyethylene ether phosphate, so that the wetting and penetrating abilities of the suspoemulsion are further improved, and the quick-acting property and the lasting property of the suspoemulsion are improved.
Further, the thickening agent is a mixture of xanthan gum and magnesium aluminum silicate with the mass ratio of 1: 1-2.5; the stabilizer is sodium benzoate; the antifreezing agent is glycol, and the thickening agent, the stabilizing agent and the antifreezing agent act together to further improve the fluidity, the dispersibility and the stability of the suspending agent.
The invention also provides a preparation method of the emamectin benzoate B2a benzoate and indoxacarb suspoemulsion, which comprises the following steps:
s1: mixing the indoxacarb, a wetting agent, a dispersing agent, a defoaming agent, a thickening agent, an antifreezing agent and 60-80% of water, and grinding to obtain an indoxacarb suspending agent;
s2: mixing the emamectin benzoate B2a, an emulsifier and the rest water to obtain an emamectin benzoate B2a aqueous emulsion;
s3: mixing the indoxacarb suspending agent with the emamectin B2a benzoate aqueous emulsion, and adding the stabilizer and the synergist to prepare the suspoemulsion.
Further, in step S1, the fineness of the grinding is less than or equal to 5 μm. The dispersibility and stability of the system are ensured.
Compared with the prior art, the preparation method of the suspension emulsion of the emamectin benzoate B2a and the indoxacarb provided by the invention takes water as a solvent, the indoxacarb suspending agent and the emamectin benzoate B2a aqueous emulsion are respectively prepared firstly, and then are mixed to prepare the suspension emulsion, so that the use of a large amount of organic solvent is avoided, and the problems of poor stability and easy caking of the emamectin benzoate in water are solved. The method has the advantages of simple process, environmental protection, safety, reliability and low cost.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
The suspending emulsion of emamectin benzoate B2a and indoxacarb comprises the following components in percentage by mass: emamectin benzoate B2 a; 20% of indoxacarb; emulsifier Zephrym 3300B 2%; wetting agent MorwetEFW 4%; 8 percent of dispersant Morwet D-425; 0.1% of xanthan gum; 0.1% of magnesium aluminum silicate; 0.5 percent of glycol; defoaming agent AF-1500 is 0.2%; 0.01 percent of sodium benzoate; 1% of isooctanol polyoxyethylene ether phosphate; the balance being water.
The preparation method of the emamectin benzoate B2a and indoxacarb suspoemulsion comprises the following steps:
s1: mixing the indoxacarb, a wetting agent Morwet EFW, a dispersing agent Morwet D-425 and 80% of water, adding a proper amount of zirconium beads, grinding, adding an antifoaming agent AF-1500, ethylene glycol, xanthan gum and magnesium aluminum silicate, and continuously grinding until D95 is less than or equal to 5 mu m to obtain the indoxacarb suspending agent;
s2: mixing the emamectin benzoate B2a, the emulsifier Zephrym 3300B and the rest water to obtain an emamectin benzoate B2a aqueous emulsion;
s3: mixing the indoxacarb suspending agent with emamectin benzoate B2a aqueous emulsion, adding the sodium benzoate and isooctyl alcohol polyoxyethylene ether phosphate, and uniformly stirring to obtain the suspending emulsion.
Example 2
The suspending emulsion of emamectin benzoate B2a and indoxacarb comprises the following components in percentage by mass: emamectin benzoate B2 a; 0.1% of indoxacarb; emulsifier Zephrym 3300B 5%; wetting agent MorwetEFW 0.5%; the dispersant Morwet D-425 is 1%; 0.3 percent of xanthan gum; 0.7 percent of magnesium aluminum silicate; 0.5 percent of glycol; defoaming agent AF-1500 is 0.2%; 0.1 percent of sodium benzoate; 1% of isooctanol polyoxyethylene ether phosphate; the balance being water.
The preparation method of the emamectin benzoate B2a and indoxacarb suspoemulsion comprises the following steps:
s1: mixing the indoxacarb, a wetting agent Morwet EFW, a dispersing agent Morwet D-425 and 60% of water, adding a proper amount of zirconium beads, grinding, adding an antifoaming agent AF-1500, ethylene glycol, xanthan gum and magnesium aluminum silicate, and continuously grinding until D95 is less than or equal to 5 mu m to obtain the indoxacarb suspending agent;
s2: mixing the emamectin benzoate B2a, the emulsifier Zephrym 3300B and the rest water to obtain an emamectin benzoate B2a aqueous emulsion;
s3: mixing the indoxacarb suspending agent with emamectin benzoate B2a aqueous emulsion, adding the sodium benzoate and isooctyl alcohol polyoxyethylene ether phosphate, and uniformly stirring to obtain the suspending emulsion.
Example 3
The suspending emulsion of emamectin benzoate B2a and indoxacarb comprises the following components in percentage by mass: 3% of methylamino abamectin B2a benzoate; indoxacarb 10 percent; emulsifier Zephrym 3300B 3%; wetting agent MorwetEFW 3%; 5% of dispersant Morwet D-425; 0.2% of xanthan gum; 0.5 percent of magnesium aluminum silicate; 0.5 percent of glycol; defoaming agent AF-1500 is 0.2%; 0.05% of sodium benzoate; 1% of isooctanol polyoxyethylene ether phosphate; the balance being water.
The preparation method of the emamectin benzoate B2a and indoxacarb suspoemulsion comprises the following steps:
s1: mixing the indoxacarb, a wetting agent Morwet EFW, a dispersing agent Morwet D-425 and 70% of water, adding a proper amount of zirconium beads, grinding, adding an antifoaming agent AF-1500, ethylene glycol, xanthan gum and magnesium aluminum silicate, and continuously grinding until D95 is less than or equal to 5 mu m to obtain the indoxacarb suspending agent;
s2: mixing the emamectin benzoate B2a, the emulsifier Zephrym 3300B and the rest water to obtain an emamectin benzoate B2a aqueous emulsion;
s3: mixing the indoxacarb suspending agent with emamectin benzoate B2a aqueous emulsion, adding the sodium benzoate and isooctyl alcohol polyoxyethylene ether phosphate, and uniformly stirring to obtain the suspending emulsion.
Example 4
The suspending emulsion of emamectin benzoate B2a and indoxacarb comprises the following components in percentage by mass: 3% of methylamino abamectin B2a benzoate; 5 percent of indoxacarb; emulsifier Zephrym 3300B 4%; wetting agent MorwetEFW 1%; 5% of dispersant Morwet D-425; 0.6 percent of xanthan gum; 0.7 percent of magnesium aluminum silicate; 0.7 percent of ethylene glycol; defoaming agent AF-1500 is 0.1%; 0.05% of sodium benzoate; isooctanol polyoxyethylene ether phosphate 0.1%; the balance being water.
The preparation method of the emamectin benzoate B2a and indoxacarb suspoemulsion comprises the following steps:
s1: mixing the indoxacarb, a wetting agent Morwet EFW, a dispersing agent Morwet D-425 and 80% of water, adding a proper amount of zirconium beads, grinding, adding an antifoaming agent AF-1500, ethylene glycol, xanthan gum and magnesium aluminum silicate, and continuously grinding until D95 is less than or equal to 5 mu m to obtain the indoxacarb suspending agent;
s2: mixing the emamectin benzoate B2a, the emulsifier Zephrym 3300B and the rest water to obtain an emamectin benzoate B2a aqueous emulsion;
s3: mixing the indoxacarb suspending agent with emamectin benzoate B2a aqueous emulsion, adding the sodium benzoate and isooctyl alcohol polyoxyethylene ether phosphate, and uniformly stirring to obtain the suspending emulsion.
Example 5
The suspending emulsion of emamectin benzoate B2a and indoxacarb comprises the following components in percentage by mass: 4% of emamectin benzoate B2 a; 20% of indoxacarb; emulsifier Zephrym 3300B 3%; wetting agent MorwetEFW 2%; the dispersant Morwet D-425 is 3%; 0.5% of xanthan gum; 0.5 percent of magnesium aluminum silicate; 0.3 percent of ethylene glycol; defoaming agent AF-1500 is 0.3%; 0.05% of sodium benzoate; isooctanol polyoxyethylene ether phosphate 2%; the balance being water.
The preparation method of the emamectin benzoate B2a and indoxacarb suspoemulsion comprises the following steps:
s1: mixing the indoxacarb, a wetting agent Morwet EFW, a dispersing agent Morwet D-425 and 60% of water, adding a proper amount of zirconium beads, grinding, adding an antifoaming agent AF-1500, ethylene glycol, xanthan gum and magnesium aluminum silicate, and continuously grinding until D95 is less than or equal to 5 mu m to obtain the indoxacarb suspending agent;
s2: mixing the emamectin benzoate B2a, the emulsifier Zephrym 3300B and the rest water to obtain an emamectin benzoate B2a aqueous emulsion;
s3: mixing the indoxacarb suspending agent with emamectin benzoate B2a aqueous emulsion, adding the sodium benzoate and isooctyl alcohol polyoxyethylene ether phosphate, and uniformly stirring to obtain the suspending emulsion.
In order to better illustrate the technical solution of the present invention, further comparison is made below by means of a comparative example and an example of the present invention.
Comparative example 1
The emamectin benzoate B2a aqueous emulsion is prepared by adopting the same amount of emamectin B2a benzoate and an emulsifier Zephrym 3300B as in example 3 and referring to the preparation method in example 3.
Comparative example 2
The indoxacarb suspending agent is prepared by adopting the same amount of indoxacarb as that in example 3, a wetting agent Morwet EFW, a dispersing agent Morwet D-425, an antifoaming agent AF-1500, ethylene glycol, xanthan gum and magnesium aluminum silicate, and referring to the preparation method in example 3.
Comparative example 3
The emamectin benzoate B2a and indoxacarb suspoemulsion is prepared by replacing isooctanol polyoxyethylene ether phosphate in example 3 with an equivalent pesticide synergist sh-l1, and preparing the emamectin benzoate B2a and indoxacarb suspoemulsion by using other components and a preparation method which are the same as those in example 3.
Comparative example 4
The suspending emulsion of emamectin benzoate B2a and indoxacarb is prepared by replacing the emulsifier Zephrym 3300B in example 3 with an equal amount of ANTAROX L-62EO/PO block copolymer emulsifier, and preparing the suspending emulsion of emamectin benzoate B2a and indoxacarb with the other components and the preparation method which are the same as those in example 3.
Comparative example 5
The emamectin benzoate and indoxacarb suspoemulsion is prepared by replacing emamectin B2a benzoate in example 3 with equivalent emamectin B1a benzoate, and preparing the other components and the preparation method in the same way as in example 3.
Comparative example 6
The invention discloses a suspending emulsion of emamectin benzoate and indoxacarb, which is selected from example 3 in a patent (CN200810038677.9) with similar dosage to that of the emamectin benzoate and indoxacarb in the example 3 of the invention, and the specific formula is as follows: 1.5% of emamectin benzoate, 10% of indoxacarb, 10% of solvent (xylene), 8% of emulsifier (EO PO block copolymer), 5% of dispersant (polyoxyethylene ether phosphate), 2% of wetting agent (nonylphenol polyoxyethylene ether), 10% of antifreeze agent (ethylene glycol), 2% of antioxidant (2, 6-di-tert-butyl-p-cresol), 3% of defoaming agent (organic silicon), 1% of anti-settling agent and the balance of water.
The formula is prepared into the emamectin benzoate suspending emulsion according to the following operation steps:
a. adding indoxacarb original drug, a dispersing agent (polyoxyethylene ether phosphate), a wetting agent (nonylphenol polyoxyethylene ether) and water into a container according to a formula proportion, and continuously stirring to prepare a suspending agent;
b. preparing an oil phase: adding the emamectin benzoate into a solvent (dimethylbenzene) according to the formula proportion, and stirring until the emamectin benzoate is completely dissolved, wherein the emamectin benzoate is used as an oil phase for standby;
c. preparing a water phase: adding an emulsifier (EO PO block copolymer), an antifreeze agent (ethylene glycol), a defoaming agent (organic silicon) and water into a container according to the formula proportion, and stirring until the materials are completely dissolved to form a uniform water phase;
d. mixing and shearing: and d, adding the prepared oil phase into the water phase, shearing, adding the indoxacarb suspending agent prepared in the step a, and shearing. And finally adding the anti-settling agent (xanthan gum), and uniformly shearing and mixing. Namely the suspending emulsion of the emamectin benzoate indoxacarb.
Comparative example 7
An emamectin benzoate and indoxacarb microcapsule suspending agent selects 10% of emamectin benzoate with the dosage similar to that of the emamectin benzoate and indoxacarb in patent (CN201711461476.5) in embodiment 3 of the invention, and embodiment 5 of the preparation method of the indoxacarb microcapsule suspending agent specifically comprises the following steps:
preparation of urea resin prepolymer: adding 6 parts by weight of urea, 15 parts by weight of formaldehyde and 23 parts by weight of deionized water into a reactor provided with a stirring device, stirring at the speed of 240r/min, then adjusting the pH to 8.0 by using 0.5mol/L NaOH solution, heating to 70 ℃, and then preserving heat for 75min to obtain a urea-formaldehyde resin prepolymer;
preparing emamectin benzoate and indoxacarb microcapsules: dissolving 4.0 parts of emamectin benzoate and 6.0 parts of indoxacarb in an ethyl acetate solution to obtain an oil phase, uniformly mixing urea-formaldehyde resin prepolymer, 18 parts of emulsifier and 52 parts of pyroligneous to obtain a water phase, pouring the water phase into a reactor, uniformly stirring, then pouring the water phase into the oil phase, rapidly stirring to form a dispersed O/W emulsion, slowly adjusting the pH to 2.5 by using 1mol/LHCl, gradually heating and curing to form a capsule, and adjusting the pH to be approximately 7 by using 2mol/L sodium hydroxide after the reaction end point is reached to obtain the emamectin benzoate and indoxacarb microcapsules;
the preparation of the mixture comprises putting 4.8 parts of diisooctyl phthalate, 3.3 parts of trans-2-hexenol, 4 parts of α -pinene, 1.2 parts of sucrose ester, 1.3 parts of hexyl acetate, 4 parts of syrup and 3.5 parts of tea saponin into a reaction kettle for high-speed shearing and mixing, wherein the shearing speed is 850r/min, and the shearing time is 6min to obtain the mixture;
preparation of emamectin benzoate and indoxacarb microcapsule suspending agent: adding the mixture, 3 parts of lignosulfonate, 4.0 parts of stabilizer, 3 parts of attractant, 3 parts of antifreeze, 3 parts of preservative, 12 parts of defoamer, 6 parts of antioxidant and 160 parts of wood vinegar into the emamectin benzoate and indoxacarb microcapsule, and uniformly mixing to obtain the emamectin benzoate and indoxacarb microcapsule suspending agent.
Comparative example 8
A patent (CN201910260160.2) 16% emamectin benzoate and indoxacarb mixed missible oil which is similar to the dosage of the emamectin benzoate and the indoxacarb in embodiment 3 of the invention is selected, and embodiment 1(6 embodiments have little difference in drug effect) in the preparation method is selected, wherein the mass ratio of the emamectin benzoate to the indoxacarb is 4:12, and the weight percentage content of the emamectin benzoate to the indoxacarb in the missible oil is 16%; the proportion of the solvent, the emulsifier and the stabilizer is 63 percent, 20 percent and 1 percent respectively.
The preparation method of the missible oil comprises the following steps:
a, compounding emamectin benzoate and indoxacarb in a mass ratio of 4:12, and then adding an environment-friendly solvent for heating and dissolving;
b, adding an emulsifier, stirring uniformly, and adding a stabilizer for blending;
c, filtering and subpackaging to obtain an emulsifiable solution product;
wherein the solvent consists of N-methyl pyrrolidone, corn oil and rosin-based oil ND-60, and the weight ratio of the N-methyl pyrrolidone: corn oil: rosin-based oil ND-60: 20: 60;
the emulsifier is composed of block polyether G5000, calcium dodecyl benzene sulfonate and diphenyl ethyl complex phenol polyoxyethylene ether, wherein the block polyether G5000: calcium dodecylbenzenesulfonate: 20-40:40-60:20-40 of diphenyl ethyl complex phenol polyoxyethylene ether;
the stabilizer is benzoic acid and BHT, and the mass ratio of the two components is 1: 4, the proportion of all the stabilizing agents in the preparation is 1 percent.
Comparative example 9
An emamectin benzoate and indoxacarb oil suspending agent is selected from patent (CN201310028378.8) which is similar to the dosage of the emamectin benzoate and indoxacarb in embodiment 3 of the invention, and embodiment 4 of the preparation method thereof, 25% of the emamectin benzoate and indoxacarb oil suspending agent comprises the following components: 5% of emamectin benzoate, 20% of indoxacarb, 2% of oleic acid polyoxyethylene ether, 5% of alkylphenol polyoxyethylene ether, 3% of castor oil polyoxyethylene ether, 2% of organic bentonite, 0.1% of triethanolamine and the balance of corn oil to 100%.
The above comparative examples do not indicate that the specific components of emamectin benzoate are all commercially available products, i.e. emamectin B1a benzoate is the main component.
To better illustrate the properties of the emamectin benzoate B2a and indoxacarb suspoemulsion provided in the examples of the present invention, the pharmaceutical preparations prepared in examples 1 to 5 and comparative examples 1 to 9 were subjected to the efficacy test.
And (3) field test: preventing and treating rice stem borer
The suspoemulsion of 3 embodiments of the invention and 8 comparative examples are used for field rice stem borer prevention and control tests, and the test method comprises the following steps: selecting a representative paddy field with flat terrain and uniform fertility level for spraying, wherein the age of the paddy field is from the early incubation period of chilo suppressalis to the 2-year worm stage, the weather is clear on the day of pesticide application, no wind and rain exist 24 hours after the test, averagely dividing the paddy field with 10 multiplied by 100 meters into 10 parts, taking one group as a control group, uniformly spraying clear water, and uniformly spraying the other 9 groups with the samples of the examples and the comparative examples respectively, wherein the using amount of the preparation is 10 ml/mu.
Data investigation: before application, uniformly selecting 5 points in each cell for sampling, taking 10 plants at each point, counting insects, and recording the age and the number of the insects. And (5) investigating the population of the insects at 1d, 3d, 7d, 14d, 21d and 30d after the application, selecting 5 points in each cell, taking 10 plants at each point, recording the number of live insects and the age of the insects, and calculating the control effect.
Insect control effect (%) (blank group having insect rate-treatment zone having insect rate) ÷ blank group having insect rate x 100
Wherein, the insect pest rate of the blank group is taken and averaged, and the experimental result is shown in table 1.
TABLE 1
As can be seen from the above table, compared with the comparative example, the examples of the present invention have better quick-acting property and long-acting property, wherein, the example 3 has excellent long-acting property and quick-acting property, the control effect can reach more than 90% 1 day after the application, and the control effect can also reach 90% 30 days after the application. The other embodiment of the present invention has an effect equivalent to that of embodiment 3. In addition, the stability of the examples and comparative examples were compared as shown in table 2.
TABLE 2
The experiment for preventing and controlling the bacterial leaf blight of rice in the field:
the rice field which has suffered from bacterial leaf blight and is in the early stage of disease is selected for carrying out pesticide effect test, the rice bacterial leaf blight is difficult to cure due to the high propagation speed of the rice bacterial leaf blight, and the disease incidence rate of the selected rice field is about 10%. The suspoemulsions of the present invention were tested in 3 examples and 8 comparative examples.
Data investigation: before drug application, sampling at 5 points uniformly in each cell, taking 100 plants at each point, performing statistics, and calculating the average. The results of the examination on days 3, 5 and 15 are shown in Table 3.
TABLE 3
As can be seen from the above table, the suspoemulsion of the present invention has a certain control effect on rice leaf blight, and other comparative examples have almost no effect on controlling bacterial blight.
In conclusion, the emamectin benzoate B2a benzoate and indoxacarb suspoemulsion provided by the invention does not use an organic solvent, has a small dosage of an auxiliary agent, has a good insecticidal effect, has a certain effect on rice leaf blight, takes effect quickly, has a long lasting period, remarkably reduces the application times, achieves the aims of lowering the application synergistic effect and preventing multiple diseases by one spraying, and has high social and economic benefits.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents or improvements made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (10)
1. The suspending emulsion of the emamectin benzoate B2a and the indoxacarb is characterized in that: comprises the following components in percentage by mass: 0.1-10% of methylamino abamectin B2a benzoate; 0.1-20% of indoxacarb; 2-5% of an emulsifier; 0.5-4% of a wetting agent; 1-8% of a dispersant; 0.1 to 1 percent of thickening agent; 0.3 to 0.7 percent of antifreeze; 0.1 to 0.3 percent of defoaming agent; 0.01-0.1% of a stabilizer; 0.1 to 2 percent of synergist; the balance being water.
2. The emamectin benzoate-indoxacarb suspoemulsion of claim 1, characterized in that: the mass ratio of the emamectin benzoate B2a to the indoxacarb is 3: 5-15.
3. The emamectin benzoate-indoxacarb suspoemulsion of claim 1, characterized in that: the wetting agent is an alkyl naphthalene sulfonate wetting agent.
4. The emamectin benzoate-indoxacarb suspoemulsion of claim 1, characterized in that: the dispersant is an alkyl naphthalene sulfonate formaldehyde condensate.
5. The emamectin benzoate-indoxacarb suspoemulsion of claim 1, characterized in that: the emulsifier is isopropyl ammonium alkyl benzene sulfonate.
6. The emamectin benzoate-indoxacarb suspoemulsion of claim 1, characterized in that: the defoaming agent is an organic silicon defoaming agent.
7. The emamectin benzoate-indoxacarb suspoemulsion of claim 1, characterized in that: the synergist is isooctanol polyoxyethylene ether phosphate.
8. The emamectin benzoate-indoxacarb suspoemulsion of claim 1, characterized in that: the thickening agent is a mixture of xanthan gum and magnesium aluminum silicate with the mass ratio of 1: 1-2.5; the stabilizer is sodium benzoate; the antifreezing agent is ethylene glycol.
9. A process for the preparation of the emamectin benzoate B2a and indoxacarb suspoemulsion according to any one of claims 1 to 8, characterized in that: the method comprises the following steps:
s1: mixing the indoxacarb, a wetting agent, a dispersing agent, a defoaming agent, a thickening agent, an antifreezing agent and 60-80% of water, and grinding to obtain an indoxacarb suspending agent;
s2: mixing the emamectin benzoate B2a, an emulsifier and the rest water to obtain an emamectin benzoate B2a aqueous emulsion;
s3: mixing the indoxacarb suspending agent with the emamectin B2a benzoate aqueous emulsion, and adding the stabilizer and the synergist to prepare the suspoemulsion.
10. The method for preparing the emamectin benzoate-indoxacarb suspoemulsion of claim 9, which is characterized in that: in step S1, the grinding fineness is less than or equal to 5 μm.
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