CN112335667B - Oil suspending agent containing isoprothiolane and propiconazole and preparation method and application thereof - Google Patents
Oil suspending agent containing isoprothiolane and propiconazole and preparation method and application thereof Download PDFInfo
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- CN112335667B CN112335667B CN201910719807.3A CN201910719807A CN112335667B CN 112335667 B CN112335667 B CN 112335667B CN 201910719807 A CN201910719807 A CN 201910719807A CN 112335667 B CN112335667 B CN 112335667B
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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
- A01N43/64—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with three nitrogen atoms as the only ring hetero atoms
- A01N43/647—Triazoles; Hydrogenated triazoles
- A01N43/653—1,2,4-Triazoles; Hydrogenated 1,2,4-triazoles
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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
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/02—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms
- A01N43/24—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with two or more hetero atoms
- A01N43/26—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with two or more hetero atoms five-membered rings
- A01N43/28—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with two or more hetero atoms five-membered rings with two hetero atoms in positions 1,3
Abstract
The invention discloses an oil suspending agent containing isoprothiolane and propiconazole, a preparation method and application thereof, wherein the oil suspending agent comprises the following components in percentage by weight: 10-40% of isoprothiolane, 5-25% of propiconazole, 5-25% of emulsifier, 2-10% of dispersant, 2-8% of wetting agent, 1-6% of thickening agent, 1-5% of stabilizer and the balance of dispersion medium to 100%. The invention compounds the isoprothiolane and the propiconazole to prepare the oil suspending agent, and the preparation has the advantages of good wetting and spreading, high permeability, high suspension rate, good dispersion, safety and environmental protection, reduces the dosage, the dosage frequency and the dosage cost, and has good effect on preventing and treating rice blast, banded sclerotial blight and other fungal diseases. Compared with the single dosage of isoprothiolane and propiconazole, the bactericidal and disease-preventing effects are obviously improved.
Description
Technical Field
The invention relates to a new formulation of isoprothiolane and propiconazole, in particular to an oil suspending agent containing isoprothiolane and propiconazole and a preparation method and application thereof, belonging to the technical field of pesticides.
Background
In recent years, rice blast has a tendency to increase year by year, and local large outbreaks are not rare and may occur in any year and any season. The rice blast occurs everywhere, and the occurrence of the blast is more in leaf parts and node parts, which can cause yield loss in different degrees after the occurrence of the blast, especially the early and serious neck blast or node blast can cause white spike and bring about dead production. The rice sheath blight disease is also called as leaf streak disease, commonly known as flower and stalk, rotten foot plague and eyebrow spot, is caused by rhizoctonia solani infection, and is mostly generated under the conditions of high temperature and high humidity. Sheath blight is seriously damaged in southern rice areas and is one of the main diseases in current rice production. The rice blast and the sheath blight are important diseases of rice, can cause great yield reduction, and can reduce the yield by 40-50% in serious cases, even the grains have no yield.
Isoprothiolane and propiconazole are commonly used bactericides in the rice planting process. Isoprothiolane, chemical name: diisopropyl-1, 3-dithiolan-a-ylmalonate, english name: isoprothiolane belongs to organic sulfur bactericides and systemic selective heterocyclic bactericides, and has special effect on rice blast. The rice plants absorb the medicament and accumulate in tissues, and are mainly concentrated on the cob and the peduncle, so that the invasion of germs into the human body is inhibited, the lipid metabolism of the germs is blocked, and the growth of the germs is inhibited. The isoprothiolane can play a role in preventing and treating simultaneously, has long lasting effect and rain wash resistance, and can also be used as a rice planthopper when being used in a large area.
Propiconazole, chemical name: 1- [2- (2, 4-dichlorophenyl) -4-propyl-1, 3-dioxolan-2-methyl ] -1 h-1, 2, 4-triazole, english name: the propiconazole is a faint yellow to light brown viscous liquid, is a systemic triazole fungicide with protection and treatment effects, can be absorbed by roots, stems and leaves, can be quickly conducted upwards in plant strains, and can be used for preventing and treating diseases caused by ascomycetes, basidiomycetes and imperfect fungi, particularly has a good prevention and treatment effect on wheat take-all, powdery mildew, rust disease, root rot, rice bakanae disease and banana leaf spot.
At present, isoprothiolane and propiconazole mainly exist in the form of emulsifiable solution, but with the increasing prominence of environmental problems, various restrictions such as various solvents used in the emulsifiable solution cause restrictions on the use of drugs, so that the development of new formulations is imperative. The oil suspending agent belongs to an environment-friendly preparation, is superior to missible oil in wetting, spreading and penetration of liquid medicine during use, and can better exert the drug effect. At present, no report related to isoprothiolane and propiconazole oil suspending agents is found.
Disclosure of Invention
The invention aims to provide an oil suspending agent containing isoprothiolane and propiconazole, which is environment-friendly, has strong permeability of a dispersion medium on plant epidermis, excellent performance in wetting spreading and permeation, high suspension rate, good dispersibility, excellent sterilization effect and convenient use.
The invention compounds the isoprothiolane and the propiconazole, and prepares the two into the oil suspending agent. After the isoprothiolane and the propiconazole are compounded, the drug effect is improved, the generation of resistance is delayed, the drug administration times and the drug administration cost are reduced, and the drug administration efficiency is obviously improved. The oil suspending agent is convenient to use, high in drug effect, environment-friendly, free of dust in the using and production processes, green, environment-friendly, time-saving, labor-saving and convenient to popularize.
The isoprothiolane and the propiconazole have good systemic property and stably exist in water environment, due to the physicochemical properties of the isoprothiolane and the propiconazole, the isoprothiolane and the propiconazole are difficult to be made into suspending agents and solid preparations and can only be made into liquid preparations, the isoprothiolane and the propiconazole are generally made into emulsifiable concentrates at present, but with the increasingly prominent environmental problems, various restrictions such as various solvents used in the emulsifiable concentrates and the like can cause limitations on the use of medicines. The invention prepares the two compounds into a new preparation form, namely an oil suspending agent, which has more advantages, but the technical problems of low melting point of raw medicines, high processing difficulty and poor stability exist in the preparation process, and the inventor solves the problems by selecting the components and the content of the auxiliary agent, particularly by matching and combining the emulsifier and the dispersant, and obtains the oil suspending agent with the conventional process, stable storage quality and high drug effect preparation performance.
Through a large number of researches and screens, the oil suspending agent containing isoprothiolane and propiconazole with stable performance is obtained, and comprises the following components in percentage by weight: 10-40% of isoprothiolane, 5-25% of propiconazole, 5-25% of emulsifier, 2-10% of dispersant, 2-8% of wetting agent, 1-6% of thickening agent, 1-5% of stabilizer and the balance of dispersion medium to 100%. The emulsifier is used for emulsifying and dispersing an oil phase carrier, the dispersant is used for playing a dispersing role to uniformly disperse small pesticide solid particles in a suspension system to avoid flocculation, the wetting agent is used for increasing the wetting and permeation of liquid medicine to a treatment object during pesticide application, the thickener is used for increasing the viscosity of the oil suspending agent to increase the physical stability, the stabilizer is used for maintaining the chemical and physical properties of the preparation in the transportation and storage processes, and the dispersion medium is used for dispersing other components except the self component in the preparation.
Further, in the oil suspending agent, the mass ratio of the isoprothiolane to the propiconazole is 1-4:1, preferably 3: 1. Within this mass ratio range, the two show better synergistic effect.
Preferably, the oil suspending agent consists of the following components in percentage by weight: 10-40% of isoprothiolane, 5-25% of propiconazole, 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.
Preferably, the oil suspending agent consists of the following components in percentage by weight: 30% of isoprothiolane, 10% of propiconazole, 15% of emulsifier, 4% of dispersant, 6% of wetting agent, 2.5% of thickening agent, 3% of stabilizer and the balance of dispersion medium being 100%. The sterilization effect is best under the condition of optimizing the proportion and the content of the effective components.
Further, in the oil suspending agent, isoprothiolane and propiconazole are used as effective components, and the total content of the two components in the oil suspending agent is 15 to 50wt%, preferably 20 to 40 wt%. Under the content range of the effective components, the components between the active components and the auxiliary agent are more stable in the system and have better drug effect.
Further, in the oil suspending agent, the emulsifier is one or more of nonylphenol polyoxyethylene ether, fatty alcohol polyoxyethylene ether, styrylphenol polyoxyethylene ether, castor oil polyoxyethylene ether, calcium dodecylbenzene sulfonate, alkylphenol formaldehyde resin polyoxyethylene ether and polyoxyethylene ether.
Further, in the oil suspending agent, the dispersant is one or more of phosphate ammonium salt, calcium lignosulfonate, sodium naphthalene sulfonate formaldehyde condensate (low naphthalene nucleus number), TERSPERSE 2020 and sodium polycarboxylate. The sodium salt of polycarboxylic acid used in the present invention may be styrene-sodium methacrylate copolymer or sodium polyacrylate.
Further, in the oil suspending agent, the wetting agent is one or more of sodium dodecyl sulfate, sodium salt of succinic acid half ester sulfonate which is an alkylphenol polyoxyethylene formaldehyde condensate, sodium lauryl alcohol ether sulfate, sodium dodecyl sulfate and nekal BX.
Further, in the oil suspending agent, the thickening agent is one or more of organic bentonite, fumed silica, xanthan gum, magnesium aluminum silicate and sodium alginate.
Further, in the oil suspending agent, the stabilizer is one or more of tributyl phosphate, butyl hydroxy anisole, triphenyl phosphite and sodium benzoate.
Further, in the oil suspension, the dispersion medium is one or more of methyl oleate, rosin-based vegetable oil, epoxidized soybean oil, paraffin oil and methyl palmitate.
Furthermore, when the auxiliary agent is optimized, the optimization of the performance of the preparation form and the drug effect exertion of the effective components are facilitated, and the performance and the drug effect exertion of the preparation form are better promoted. Preferably, the emulsifier is formed by mixing fatty alcohol polyoxyethylene ether (AEO-9) and castor oil polyoxyethylene ether (LCN-40) according to the mass ratio of 1: 1-3. Preferably, the dispersant is prepared by mixing phosphate ammonium salt and TERSPERSE 2020 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 thickener is prepared 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. Through the optimization and combination of all the auxiliary agents, particularly the combination of the fatty alcohol polyoxyethylene ether (AEO-9) auxiliary agent and the phosphate ammonium salt auxiliary agent, the stability of the preparation is improved, and the processing difficulty of the preparation is reduced.
Experiments prove that the oil suspending agent provided by the invention has the advantages of less residue after pouring, good dispersion stability, high suspension rate, good thermal stability and strong adhesive force, can better play the synergistic effect of active ingredients, greatly improves the sterilization rate, can effectively prevent and remove rice blast and sheath blight of rice, is convenient to use, can be used for conventional spraying and spraying of plant protection unmanned aerial vehicles, and has the advantages of difficult volatilization of liquid medicine, drift resistance, strong wetting and spreading performance, good permeation conductivity and rain wash resistance.
The invention also provides a preparation method of the 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, isoprothiolane and propiconazole into a reaction kettle under high-speed shearing, shearing for 10-35 minutes, and then grinding until the particle size D of the mixture is reached90And (5) the suspension concentrate is less than 5 mu m to obtain the oil suspension concentrate containing isoprothiolane and propiconazole.
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.
The invention prepares the isoprothiolane and the propiconazole into the oil suspending agent by compounding, the preparation formulation can be suitable for the dispersion and the exertion of the isoprothiolane and the propiconazole simultaneously, the drug effect is effectively improved, and compared with the preparation formulations such as missible oil, powder, suspending agent and the like, the preparation formulation has the advantages of strong dispersion stability, strong adhesiveness and permeability, convenient use, no dust in the preparation and process, more environment-friendly auxiliary agent and difficult pollution to the environment, people and livestock. Therefore, the application of the oil suspending agent containing isoprothiolane and propiconazole in preventing and treating rice blast or sheath blight of rice is also within the protection range.
The invention has the following beneficial effects:
1. the composition has high safety to rice crops and has good synergistic and complementary effects, so that the bactericidal spectrum is increased, the pesticide effect is high compared with the single dosage of the isoprothiolane and the propiconazole, the pesticide dosage and the pesticide use times are reduced, the agricultural production cost is saved, and the bactericidal effect is obviously improved.
2. The invention prepares the isoprothiolane and the propiconazole into the oil suspending agent, 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 oil suspending agent has the advantages of less pouring residue, good emulsifying dispersibility, high suspension rate, good heat storage stability and the like, and effectively solves the problems of large oil precipitation or caking, large particle size growth and the like in sample storage.
3. The oil suspending agent has the advantages of simple preparation process, easy operation, convenient processing and use, no dust pollution, environmental protection, time saving and labor saving. The liquid medicine is not easy to volatilize, is resistant to drift, has strong wetting and spreading performance, good permeation conductivity, strong epidermis permeability and rain wash resistance, has strong adhesiveness and permeability compared with dosage forms such as missible oil, powder, aqueous suspension and the like, and improves the sterilization effect.
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% isoprothiolane-propiconazole oil suspension
The formula is as follows: the effective components of isoprothiolane 10%, propiconazole 5%, emulsifier nonylphenol polyoxyethylene ether 2%, styrylphenol polyoxyethylene ether 3%, dispersant calcium lignosulfonate 2%, sodium naphthalene sulfonate formaldehyde condensate (low naphthalene nucleus number) 1%, wetting agent sodium dodecyl sulfate 1%, thickener sodium alginate 2%, magnesium aluminum silicate 4%, stabilizer tributyl phosphate 2%, and the balance of dispersion medium methyl palmitate.
The preparation method comprises the following steps: adding an emulsifier, a dispersant, a wetting agent and a stabilizer into a dispersion medium, adding the emulsifier, the dispersant, the wetting agent and the stabilizer into a reaction kettle with a shearing device, and fully mixing, emulsifying and uniformly dispersing; adding the thickening agent, isoprothiolane and propiconazole into the reaction kettle under the high-speed shearing state (2500-90Until the grain size is less than 5 mu m, obtaining 15 percent isoprothiolane-propiconazoleAn oil suspending agent.
Example 220% isoprothiolane-propiconazole oil suspension
The formula is as follows: the effective components of isoprothiolane 10%, propiconazole 10%, emulsifier castor oil polyoxyethylene ether (LCN-40) 5%, fatty alcohol polyoxyethylene ether (AEO-9) 5%, dispersant phosphate ammonium salt 6.4%, TERSPERSE 20201.6%, wetting agent alkylphenol polyoxyethylene ether formaldehyde condensate succinic acid half ester sulfonic acid sodium salt 1.5%, nekal BX1.5%, thickener fumed silica 1%, organic bentonite 1%, stabilizer butyl hydroxy anisole 2%, and the balance of dispersion medium methyl oleate. The preparation method is the same as example 1.
Example 330% isoprothiolane propiconazole oil suspension
The formula is as follows: the effective components of isoprothiolane 20%, propiconazole 10%, emulsifier castor oil polyoxyethylene ether (LCN-40) 15%, fatty alcohol polyoxyethylene ether (AEO-9) 5%, dispersant phosphate ammonium salt 4%, TERSPERSE 20202%, wetting agent alkylphenol polyoxyethylene ether formaldehyde condensate succinic acid half ester sulfonic acid sodium salt 1%, nekal BX 2%, thickener fumed silica 2%, organic bentonite 3%, stabilizer butyl hydroxy anisole 3%, and the balance of dispersion medium methyl oleate. The preparation method is the same as example 1.
Example 440% isoprothiolane-propiconazole oil suspension
The formula is as follows: the effective components of isoprothiolane 30%, propiconazole 10%, emulsifier castor oil polyoxyethylene ether (LCN-40) 10%, fatty alcohol polyoxyethylene ether (AEO-9) 5%, dispersant phosphate ammonium salt 2%, TERSPERSE 20202%, wetting agent alkylphenol polyoxyethylene ether formaldehyde condensate succinic acid half ester sulfonic acid sodium salt 1.5%, nekal BX4.5%, thickener fumed silica 0.5%, organic bentonite 2%, stabilizer butyl hydroxy anisole 3%, and the balance of dispersion medium methyl oleate. The preparation method is the same as example 1.
Example 540% isoprothiolane-propiconazole oil suspension
The formula is as follows: the effective components of isoprothiolane 20%, propiconazole 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% isoprothiolane propiconazole oil suspension
The formula is as follows: the effective components of isoprothiolane 35%, propiconazole 10%, emulsifier alkylphenol formaldehyde resin polyoxyethylene ether 10%, fatty alcohol polyoxyethylene ether (AEO-9) 15%, dispersant calcium lignosulfonate 4%, sodium naphthalene sulfonate formaldehyde condensate (low naphthalene nucleus number) 2%, wetting agent sodium laureth sulfate 3%, sodium dodecyl sulfate 5%, thickener magnesium aluminum silicate 3%, sodium alginate 2%, stabilizer triphenyl phosphite 2%, and the balance of dispersion medium rosin-based vegetable oil. The preparation method is the same as example 1.
Example 750% isoprothiolane-propiconazole oil suspension
The formula is as follows: the effective components of isoprothiolane 40%, propiconazole 10%, emulsifier castor oil polyoxyethylene ether (LCN-40) 12%, fatty alcohol polyoxyethylene ether (AEO-9) 6%, dispersant phosphate ammonium salt 2%, TERSPERSE 20201%, wetting agent alkylphenol polyoxyethylene ether formaldehyde condensation succinic acid half ester sulfonic acid sodium salt 2%, nekal BX 3%, thickener fumed silica 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% isoprothiolane propiconazole oil suspension
The formula is as follows: the effective components of isoprothiolane 25%, propiconazole 10%, emulsifier nonylphenol polyoxyethylene ether 12%, styrylphenol polyoxyethylene ether 5%, dispersing agent TERSPERSE 20206%, calcium lignosulphonate 4%, wetting agent nekal BX 5%, sodium dodecyl sulfate 1%, thickening agent xanthan gum 2%, sodium alginate 2%, stabilizing agent triphenyl phosphite 5%, and the balance of dispersing medium paraffin oil. The preparation method is the same as example 1.
Comparative example 30% isoprothiolane-propiconazole oil suspending agent
The formula is as follows: the effective components of isoprothiolane 20%, propiconazole 10%, emulsifier polysorbate 15%, calcium dodecylbenzene sulfonate 5%, dispersant ethylene oxide-propylene oxide block copolymer 5%, sodium methylene dinaphthalene sulfonate 1%, wetting agent fatty alcohol polyoxyethylene ether sodium sulfate 3%, thickener carboxymethyl cellulose 2%, diatomite 3%, stabilizer triphenyl phosphite 3%, and the balance of epoxidized soybean oil. The preparation method is the same as example 1.
The performance of the oil suspending agents prepared in the above examples and comparative examples was 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.
As can be seen from Table 1, the oil suspending agent obtained in the examples of the present invention has low residue on dumping, excellent dispersion and emulsification properties, satisfactory appearance, a suspension rate of the agent of 90% or more, and good stability after thermal storage. Examples 1, 5, 6, and 8 were slightly inferior in quality after heat storage but met the quality requirements, and examples 2 to 4, and 7 were excellent in quality both before and after heat storage. However, the comparative examples show the phenomenon that the pouring residue has high influence on the use, and the indexes of dispersion emulsibility, appearance and suspension rate are generally slightly poor. It can be seen that the preferred auxiliaries play a critical role in the product quality.
As can be seen from examples 2-4 and example 7, the properties of the oil suspensions obtained with varying amounts of the pharmaceutically active ingredient in the range of 20-50% were similar with the selection of the preferred adjuvants, indicating that the drug content had less effect on the dosage form properties with the preferred adjuvant ingredients and amounts. As can be seen from examples 1, 5, 6 and 8, in the case of the conventional adjuvant, the performance of the obtained oil suspending agent is relatively poor, and the replacement adjuvant has no obvious effect improvement, which shows that the components and content of the preferable adjuvant have obvious improvement effect on the performance of the isoprothiolane-propiconazole oil suspending agent, and the conventional adjuvant does not exist.
Field test example 1: pesticide effect test for preventing and controlling rice blast in field test
The test is arranged to be carried out in Changsha city, Hunan province, and the contrast agents are 40% isoprothiolane missible oil (purchased from the market) and 25% propiconazole missible oil (purchased from the market). The total number of 4 treatments are respectively as follows: treatment 1: spraying clear water, and blank control; and (3) treatment 2: the isoprothiolane-propiconazole oil suspensions obtained in examples 1 to 8 and comparative example; and (3) treatment: 40% isoprothiolane emulsifiable concentrate; and (4) treatment: 25% propiconazole emulsifiable concentrate.
Wherein, the isoprothiolane-propiconazole oil suspension obtained in examples 1 to 8 and comparative example was subjected to stem and leaf spray treatment with an effective ingredient usage of 380 g/hectare, treatment 3 was subjected to stem and leaf spray treatment with an effective ingredient usage of 800 g/hectare, and treatment 4 was subjected to stem and leaf spray treatment with an effective ingredient usage of 150 g/hectare.
Experiments are carried out in a direct rice seeding field, the rice is in a heading stage, and the depth of a water layer in the field is about 6 cm. The experimental plot is divided into a plurality of cells, and ridges are arranged among the cells to block the cells. The test cells are randomly arranged, blank control treatment and medicament treatment are set in the test, 12 groups of treatment are totally set, and each treatment is repeated for 3 times.
The blast disease was in the stage of development during the test. The pesticide is applied for 1 time by a worker-farm-16 knapsack manual sprayer, 600kg of water is added to prepare the 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 25-35.0 ℃. There was no rain on the day of application. The investigation method refers to GB/T17980.19-2000, and investigation is carried out before and 14 days after the medicine, and the prevention and treatment effect is calculated.
The control effect calculation method comprises the following steps:
the disease index of the control area is the disease index of the blank control area, and no medicament is sprayed.
During the test, the compound preparation of the invention has no adverse effect on rice in the test application range, and the test results are as follows:
as can be seen from Table 2, the rice blast can be effectively prevented and controlled after the isoprothiolane and the propiconazole are compounded, and the prevention and control effects are superior to those of a control medicament. Wherein, the control effect of the embodiment using the preferred auxiliary agent is obviously better than that of other embodiments and comparative examples, and the control effect on the rice blast is more than 90 percent; the control effect of other examples and comparative examples is more than 78 percent and is also better than that of a control medicament.
Field test example 2: pesticide effect test for preventing and controlling rice sheath blight disease in field test
The test is arranged to be carried out in Changsha city, Hunan province, and the contrast agents are 40% isoprothiolane missible oil (purchased from the market) and 25% propiconazole missible oil (purchased from the market). The total number of 4 treatments are respectively as follows: treatment 1: spraying clear water, and blank control; and (3) treatment 2: the isoprothiolane-propiconazole oil suspensions obtained in examples 1 to 8 and comparative example; and (3) treatment: 40% isoprothiolane emulsifiable concentrate; and (4) treatment: 25% propiconazole emulsifiable concentrate.
Wherein, the isoprothiolane-propiconazole oil suspension obtained in examples 1 to 8 and comparative example was subjected to stem and leaf spray treatment with an effective ingredient usage of 380 g/hectare, treatment 3 was subjected to stem and leaf spray treatment with an effective ingredient usage of 800 g/hectare, and treatment 4 was subjected to stem and leaf spray treatment with an effective ingredient usage of 150 g/hectare.
Experiments are carried out in a direct rice seeding field, the rice is in a heading stage, and the depth of a water layer in the field is about 6 cm. The experimental plot is divided into a plurality of cells, and ridges are arranged among the cells to block the cells. The test cells are randomly arranged, blank control treatment and medicament treatment are set in the test, 12 groups of treatment are totally set, and each treatment is repeated for 3 times.
The sheath blight disease was in the onset stage during the test. The pesticide is applied for 1 time by a worker-farm-16 knapsack manual sprayer, 600kg of water is added to prepare the 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 25-35.0 ℃. There was no rain on the day of application. The investigation method refers to GB/T17980.19-2000, and investigation is carried out before and 14 days after the medicine, and the prevention and treatment effect is calculated.
The control effect calculation method comprises the following steps:
the disease index of the control area is taken as the disease index of the blank control area, and no medicament is sprayed.
During the test, the compound preparation of the invention has no adverse effect on rice in the test application range, and the test results are as follows:
as can be seen from Table 3, the rice blast and propiconazole can effectively prevent and treat the rice sheath blight disease after being compounded, and the prevention and treatment effects are superior to those of a control medicament. Wherein, the control effect of the embodiment using the preferred auxiliary agent is obviously better than that of other embodiments and comparative examples, and the control effect on rice sheath blight is more than 90%; the control effect of other examples and comparative examples is more than 80 percent and is also better than that of a control medicament.
Claims (10)
1. An oil suspending agent containing isoprothiolane and propiconazole, which is characterized in that: the composition comprises the following components in percentage by weight: 10-40% of isoprothiolane, 5-25% of propiconazole, 5-25% of emulsifier, 2-10% of dispersant, 2-8% of wetting agent, 1-6% of thickening agent, 1-5% of stabilizer and the balance of dispersion medium being 100%;
the emulsifier is one or more of nonylphenol polyoxyethylene ether, fatty alcohol polyoxyethylene ether, styrylphenol polyoxyethylene ether, castor oil polyoxyethylene ether, calcium dodecylbenzene sulfonate, alkylphenol formaldehyde resin polyoxyethylene ether and polyoxyethylene ether; the dispersant is one or more of phosphate ammonium salt, calcium lignosulfonate, sodium naphthalene sulfonate formaldehyde condensate, TERSPERSE 2020 and sodium polycarboxylate; the wetting agent is one or more of sodium dodecyl sulfate, sodium salt of succinic acid half ester sulfonate which is an alkylphenol polyoxyethylene formaldehyde condensate, sodium lauryl ether sulfate, sodium dodecyl sulfate and nekal BX.
2. The oil suspension as set forth in claim 1, characterized in that: the composition comprises the following components in percentage by weight: 10-40% of isoprothiolane, 5-25% of propiconazole, 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%.
3. The oil suspending agent according to claim 1 or 2, characterized in that: the mass ratio of the isoprothiolane to the propiconazole is 1-4: 1.
4. The oil suspension as set forth in claim 3, characterized in that: the mass ratio of the isoprothiolane to the propiconazole is 3: 1.
5. The oil suspending agent according to claim 1 or 2, characterized in that: the total content of isoprothiolane and propiconazole in the oil suspending agent is 15-50 wt%.
6. The oil suspension as set forth in claim 2, characterized in that: the composition comprises the following components in percentage by weight: 30% of isoprothiolane, 10% of propiconazole, 15% of emulsifier, 4% of dispersant, 6% of wetting agent, 2.5% of thickening agent, 3% of stabilizer and the balance of dispersion medium being 100%.
7. The oil suspension as set forth in claim 1, characterized in that: the thickening agent is one or more of organic bentonite, fumed silica, xanthan gum, magnesium aluminum silicate and sodium alginate; the stabilizer is one or more of tributyl phosphate, butyl hydroxy anisole, triphenyl phosphite and sodium benzoate; the dispersion medium is one or more of methyl oleate, rosin-based vegetable oil, epoxidized soybean oil, paraffin oil and methyl palmitate.
8. The oil suspension as set forth in claim 1, characterized in that: the emulsifier is formed by mixing fatty alcohol-polyoxyethylene ether and castor oil-polyoxyethylene ether according to the mass ratio of 1: 1-3; the dispersing agent is formed by mixing phosphate ammonium salt and TERSPERSE 2020 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.
9. A method for producing the oil suspending agent containing isoprothiolane and propiconazole according to any one of claims 1 to 8, which is characterized by comprising the steps of:
(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, isoprothiolane and propiconazole into a reaction kettle under high-speed shearing, shearing for 10-35 minutes, and then grinding until the particle size D of the mixture is reached90And (5) the suspension concentrate is less than 5 mu m to obtain the oil suspension concentrate containing isoprothiolane and propiconazole.
10. The use of the oil suspending agent containing isoprothiolane and propiconazole according to any one of claims 1 to 8 for controlling fungal diseases of rice, characterized in that: the disease is rice blast or sheath blight.
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| CN101433203A (en) * | 2008-12-05 | 2009-05-20 | 浙江禾本农药化学有限公司 | Plant bactericidal composition and uses thereof |
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| CN104719306A (en) * | 2015-03-25 | 2015-06-24 | 山东潍坊润丰化工股份有限公司 | Fungicidal composition containing isoprothiolane and propiconazole and application of fungicidal composition |
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