Bactericide composition containing triphenyltin acetate and difenoconazole and preparation method thereof
阅读说明：本技术 一种含三苯基乙酸锡与苯醚甲环唑杀菌剂组合物及其制备方法 (Bactericide composition containing triphenyltin acetate and difenoconazole and preparation method thereof ) 是由 张青华 王进 徐瑶 李雪芬 潘光飞 陈华 金晓恩 唐银东 曾挺 于 2020-12-17 设计创作，主要内容包括：本发明公开了一种三苯基乙酸锡与苯醚甲环唑杀菌剂组合物及其制备方法,该组合物将三苯基乙酸锡和苯醚甲环唑进行复配,具有很好的协同增效作用,其中三苯基乙酸锡与苯醚甲环唑的重量比为1:10至10:1。本发明组合物扩大了杀菌谱,提高杀菌效率,避免了病害的抗药性,延长了药物持效期,在防农作物的白粉病、黑星病、斑点落叶病等病害中有很好的效果。(The invention discloses a triphenyltin acetate and difenoconazole bactericide composition and a preparation method thereof, the composition is prepared by compounding triphenyltin acetate and difenoconazole, and has a good synergistic interaction effect, wherein the weight ratio of the triphenyltin acetate to the difenoconazole is 1: 10-10: 1. The composition of the invention expands the bactericidal spectrum, improves the bactericidal efficiency, avoids the drug resistance of diseases, prolongs the drug effect duration, and has good effect in preventing diseases of crops such as powdery mildew, scab, alternaria leaf spot and the like.)
1. The bactericide composition containing the triphenyltin acetate and the difenoconazole is characterized by comprising the following components in percentage by weight: 1-80% of active ingredients of the medicine and the balance of auxiliary materials; the active ingredients of the medicine comprise the following components in percentage by weight (1: 10): (10:1) difenoconazole and triphenyltin acetate.
2. The bactericidal composition containing triphenyltin acetate and difenoconazole according to claim 1, wherein the pharmaceutical active ingredients comprise (1:1) by weight: (5:1) difenoconazole and triphenyltin acetate.
3. The bactericidal composition containing triphenyltin acetate and difenoconazole according to claim 1, wherein the dosage form of the bactericidal composition containing triphenyltin acetate and difenoconazole is any one of wettable powder, water dispersible granules, aqueous emulsion, dispersible oil suspending agent and missible oil.
4. The bactericidal composition containing triphenyltin acetate and difenoconazole according to claim 3, wherein when the dosage form of the bactericidal composition containing triphenyltin acetate and difenoconazole is wettable powder, the bactericidal composition comprises the following components in percentage by weight: 1-80% of active pharmaceutical ingredient, 1-10% of dispersant, 1-10% of wetting agent and the balance of filler; the dispersing agent is formed by mixing sodium naphthalene sulfonate and sodium lignosulfonate according to the mass ratio of 1-3: 1; the wetting agent is formed by mixing sodium dodecyl sulfate and sodium lignin sulfonate according to the mass ratio of 0.5-1.5: 1; the filler is 10-40% of white carbon black and 60-90% of talcum powder.
5. The bactericidal composition containing triphenyltin acetate and difenoconazole according to claim 4, which is characterized by comprising the following components in percentage by weight: 30-70% of active pharmaceutical ingredients, 4-8% of dispersing agent, 1-3% of wetting agent and the balance of filler.
6. The bactericidal composition containing triphenyltin acetate and difenoconazole according to claim 3, wherein when the dosage form of the bactericidal composition containing triphenyltin acetate and difenoconazole is dispersible oil suspending agent, organic solvent is used as medium, and the content of each component is as follows: 1-60% of active ingredients of the medicine, 0-20% of wetting agent, 0-20% of dispersing agent, 0.2-20% of emulsifying agent, 0-10% of suspending aid and the balance of dispersing medium; the wetting agent is sodium dodecyl sulfate; the emulsifier is formed by mixing calcium dodecyl benzene sulfonate and castor oil polyoxyethylene ether according to the ratio of 1: 0.5-2; the dispersing agent is formed by mixing an alkylphenol polyoxyethylene ether formaldehyde condensate and fatty alcohol polyoxyethylene ether sulfate according to the ratio of 10: 4-15; the suspension auxiliary agent is formed by mixing white carbon black and organic bentonite according to a ratio of 1: 1; the dispersion medium is methyl oleate.
7. The bactericidal composition containing triphenyltin acetate and difenoconazole according to claim 6, which is characterized in that the bactericidal composition containing triphenyltin acetate and difenoconazole contains the following components in percentage by weight: 20-50% of active ingredients of the medicine, 1-5% of wetting agent, 2-8% of dispersing agent, 2-8% of emulsifying agent, 1-5% of suspension aid and the balance of dispersing medium.
8. The triphenyltin acetate and difenoconazole-containing bactericide composition as claimed in claim 1, further comprising: 1.2-3.2% of chitosan oligosaccharide, 0.4-1.2% of andrographis paniculata extract, 0.2-2.5% of folium artemisiae argyi extract, 0.4-1.6% of phellodendron extract and 0.2-1.2% of brassinolide.
9. A method for preparing a fungicidal composition containing triphenyltin acetate and difenoconazole according to claim 6, which comprises the following steps: adding the pharmaceutical active ingredients, the wetting agent, the dispersing agent, the emulsifier, the suspension auxiliary agent and the dispersion medium in percentage into a feeding kettle, and stirring and shearing for 20-40 minutes to obtain a suspension; and sanding the suspension until the particle size is 4-5 mu m to obtain the bactericidal agent composition containing the triphenyltin acetate and the difenoconazole.
10. The bactericidal composition containing triphenyltin acetate and difenoconazole according to any one of claims 1-9, wherein the bactericidal composition containing triphenyltin acetate and difenoconazole is applied to prevention and treatment of scab, alternaria leaf spot, late blight, downy mildew, rust disease, powdery mildew, banded sclerotial blight and gibberellic disease of vegetables and fruit trees.
Technical Field
The invention relates to the technical field of pesticide bactericides, and particularly relates to a bactericide composition containing triphenyltin acetate and difenoconazole and a preparation method thereof.
Background
Triphenyltin acetate (also known as Triphenyltin acetate) is a white odorless crystalline powder having a melting point between 118 and 122 ℃, a solubility in water of 28ppm (20 ℃), is sparingly soluble in most organic solvents, is stable when stored in dry conditions, decomposes relatively readily when exposed to air and sunlight, and forms insoluble tin compounds. The triphenyl tin acetate has little phytotoxicity to plants and is quickly decomposed into element tin under the action of ultraviolet rays.
Difenoconazole is a low-toxicity heterocyclic bactericide pesticide with the chemical formula of C19H17Cl2N3O3The difenoconazole technical material is offwhite powder with the density of 1.40g/cm3Melting point 76.0 ℃, solubility in water of 3.3mg/L (20 ℃), is readily soluble in organic solvents, and is less mobile in soil and slowly degrades. The difenoconazole is systemic bactericide with broad bactericidal spectrum, and can be used for ascomycetes, basidiomycetes and fungi including Alternaria, Septoria, Cercospora and NitrariaThe bactericide has lasting protection and treatment effects on semi-known diseases including the genera of discodermia, acne, phoma, septoria and cladosporium, powdery mildew, rust fungales and certain species-borne pathogenic bacteria, and also has good effects on grape anthracnose and white rot. The use of difenoconazole for treating leaf surfaces or seeds can improve the yield of crops and ensure the quality of the crops.
Chinese patent CN106561670A discloses a compound composition containing clofentezine and triphenyltin acetate, which is prepared by compounding effective components of lachlor mite, clofentezine and triphenyltin acetate according to the weight ratio of 15-20: 8-12: 1-3. However, the compound composition prepared by the patent has poor compounding effect.
Disclosure of Invention
In view of the above, the invention provides a bactericide composition containing triphenyltin acetate and difenoconazole and a preparation method thereof, so as to solve the technical problems.
In order to achieve the purpose, the invention provides the following technical scheme: a bactericide composition containing triphenyltin acetate and difenoconazole, which consists of the following components in percentage by weight: 1-80% of active ingredients of the medicine and the balance of auxiliary materials; the active ingredients of the medicine comprise the following components in percentage by weight (1: 10): (10:1) difenoconazole and triphenyltin acetate.
Further, the active ingredients of the medicine comprise the following components in weight ratio (1: 1): (5:1) difenoconazole and triphenyltin acetate.
Furthermore, the dosage form of the bactericide composition is any one of wettable powder, water dispersible granules, aqueous emulsion, dispersible oil suspending agent and missible oil.
Furthermore, when the dosage form of the bactericide composition is wettable powder, the bactericide composition consists of the following components in percentage by weight: 1-80% of active pharmaceutical ingredient, 1-10% of dispersant, 1-10% of wetting agent and the balance of filler; the dispersing agent is formed by mixing sodium naphthalene sulfonate and sodium lignosulfonate according to the mass ratio of 1-3: 1; the wetting agent is formed by mixing sodium dodecyl sulfate and sodium lignin sulfonate according to the mass ratio of 0.5-1.5: 1; the filler is 10-40% of white carbon black and 60-90% of talcum powder.
More particularly, the bactericide composition consists of the following components in percentage by weight: 30-70% of active pharmaceutical ingredients, 4-8% of dispersing agent, 1-3% of wetting agent and the balance of filler.
Furthermore, when the dosage form of the bactericide composition is a dispersible oil suspending agent, the bactericide composition takes an organic solvent as a medium, and comprises the following components in percentage by weight: 1-60% of active ingredients of the medicine, 0-20% of wetting agent, 0-20% of dispersing agent, 0.2-20% of emulsifying agent, 0-10% of suspending aid and the balance of dispersing medium; the wetting agent is sodium dodecyl sulfate; the emulsifier is formed by mixing calcium dodecyl benzene sulfonate and castor oil polyoxyethylene ether according to the ratio of 1: 0.5-2; the dispersing agent is formed by mixing an alkylphenol polyoxyethylene ether formaldehyde condensate and fatty alcohol polyoxyethylene ether sulfate according to the ratio of 10: 4-15; the suspension auxiliary agent is formed by mixing white carbon black and organic bentonite according to a ratio of 1: 1; the dispersion medium is methyl oleate.
More particularly, the bactericide composition comprises the following components in percentage by weight: 20-50% of active ingredients of the medicine, 1-5% of wetting agent, 2-8% of dispersing agent, 2-8% of emulsifying agent, 1-5% of suspension aid and the balance of dispersing medium.
Further, the above-mentioned fungicide composition further comprises: 1.2-3.2% of chitosan oligosaccharide, 0.4-1.2% of andrographis paniculata extract, 0.2-2.5% of folium artemisiae argyi extract, 0.4-1.6% of phellodendron extract and 0.2-1.2% of brassinolide. Wherein the common andrographis herb extract, the folium artemisiae argyi extract and the cortex phellodendri extract are obtained by extracting through a conventional extraction method; the natural bactericidal substance is added, so that the addition amount of active ingredients of the medicine can be reduced, the pollution to the environment and soil is reduced, and the generation of drug resistance can be reduced.
The invention also aims to provide a preparation method of the bactericidal agent composition containing the triphenyltin acetate and the difenoconazole, which comprises the following steps: adding the pharmaceutical active ingredients, the wetting agent, the dispersing agent, the emulsifier, the suspension auxiliary agent and the dispersion medium in percentage into a feeding kettle, and stirring and shearing for 20-40 minutes to obtain a suspension; and sanding the suspension until the particle size is 4-5 mu m to obtain the bactericidal agent composition containing the triphenyltin acetate and the difenoconazole.
The invention also aims to provide application of the bactericide composition containing the triphenyl tin acetate and the difenoconazole in preventing and treating scab, alternaria leaf spot, late blight, downy mildew, rust disease, powdery mildew, banded sclerotial blight and gibberellic disease of vegetables and fruit trees.
The technical scheme can show that the invention has the advantages that:
1. according to the bactericide composition containing the triphenyltin acetate and the difenoconazole, the triphenyltin acetate and the difenoconazole are reasonably compounded to realize the effects of expanding the bactericidal spectrum and prolonging the effective period, and a proper amount of natural extract is added, so that the bactericidal range is expanded, the use amount of the bactericide composition is reduced, and the product is safer and more environment-friendly;
2. the dispersible oil suspending agent containing the triphenyltin acetate and difenoconazole bactericide composition prepared by the invention has the advantages of high suspension rate, strong heat storage stability, good adhesion of wettable powder on vegetables and fruit trees, high drug effect, long acting time, quick response, high prevention effect, long drug effect time, low drug usage amount, reduced planting cost, reduced harm to the environment and crops, and environmental protection and safety of the fruits and the vegetables, and the bactericide composition of two dosage forms adheres and spreads on the vegetables or the fruit trees, the insect bodies and the pathogenic bacteria.
In addition to the objects, features and advantages described above, other objects, features and advantages of the present invention are also provided. The present invention will be described in further detail below.
Detailed Description
The following detailed description of embodiments of the invention, but the invention can be practiced in many different ways, as defined and covered by the claims.
Example 1
Bactericide composition containing triphenyltin acetate and difenoconazole and preparation method thereof
The dosage form of the bactericide composition is wettable powder and consists of the following components in percentage by weight: 1% of a pharmaceutical active ingredient, 10% of a dispersing agent, 10% of a wetting agent and the balance of a filler, wherein the pharmaceutical active ingredient comprises difenoconazole and triphenyltin acetate in a weight ratio of 1: 10; the dispersing agent is formed by mixing sodium naphthalene sulfonate and sodium lignosulfonate according to the mass ratio of 1: 1; the wetting agent is prepared by mixing sodium dodecyl sulfate and sodium lignin sulfonate according to the mass ratio of 0.5: 1; the filler is 10% of white carbon black and 90% of talcum powder.
The bactericide composition containing the triphenyltin acetate and the difenoconazole is prepared by the following method: crushing the fillers in percentage by weight by using a crusher, and sieving the crushed fillers with a 325-mesh sieve; and (2) sequentially putting the filler, the dispersing agent, the wetting agent and the pharmaceutical active ingredients into a stirring container according to the mass percentage, stirring for 20 minutes, crushing the product, sieving by using a 30-55 nm sieve, crushing for 35 minutes by using a jet mill, cooling the product, detecting and packaging to obtain the finished product.
Example 2
Bactericide composition containing triphenyltin acetate and difenoconazole and preparation method thereof
The dosage form of the bactericide composition is wettable powder and consists of the following components in percentage by weight: 80% of a pharmaceutical active ingredient, 1% of a dispersing agent, 1% of a wetting agent and the balance of a filler, wherein the pharmaceutical active ingredient comprises difenoconazole and triphenyltin acetate in a weight ratio of 1: 5; the dispersing agent is formed by mixing sodium naphthalene sulfonate and sodium lignosulfonate according to the mass ratio of 3: 1; the wetting agent is prepared by mixing sodium dodecyl sulfate and sodium lignin sulfonate according to the mass ratio of 1.5: 1; the filler is 40% of white carbon black and 60% of talcum powder.
The bactericide composition containing the triphenyltin acetate and the difenoconazole is prepared by the following method: crushing the fillers in percentage by weight by using a crusher, and sieving the crushed fillers with a 325-mesh sieve; and (2) sequentially putting the filler, the dispersing agent, the wetting agent and the pharmaceutical active ingredients into a stirring container according to the mass percentage, stirring for 30 minutes, crushing the product, sieving by a 30-55 nm sieve, crushing for 30 minutes by a jet mill, cooling the product, detecting and packaging to obtain the finished product.
Example 3
Bactericide composition containing triphenyltin acetate and difenoconazole and preparation method thereof
The dosage form of the bactericide composition is wettable powder, and the bactericide composition comprises the following components in percentage by weight: 30% of a pharmaceutical active ingredient, 4% of a dispersing agent, 3% of a wetting agent and the balance of a filler, wherein the pharmaceutical active ingredient comprises difenoconazole and triphenyltin acetate in a weight ratio of 1: 1; the dispersing agent is formed by mixing sodium naphthalene sulfonate and sodium lignosulfonate according to the mass ratio of 2: 1; the wetting agent is prepared by mixing sodium dodecyl sulfate and sodium lignosulphonate according to the mass ratio of 1: 1; the filler is 20% of white carbon black and 80% of talcum powder.
The bactericide composition containing the triphenyltin acetate and the difenoconazole is prepared by the following method: crushing the fillers in percentage by weight by using a crusher, and sieving the crushed fillers with a 325-mesh sieve; and (2) sequentially putting the filler, the dispersing agent, the wetting agent and the pharmaceutical active ingredients into a stirring container according to the mass percentage, stirring for 40 minutes, crushing the product, sieving by a 30-55 nm sieve, crushing for 40 minutes by a jet mill, cooling the product, detecting and packaging to obtain the finished product.
Example 4
Bactericide composition containing triphenyltin acetate and difenoconazole and preparation method thereof
The dosage form of the bactericide composition is wettable powder, and the bactericide composition comprises the following components in percentage by weight: 70% of pharmaceutical active ingredient, 8% of dispersing agent, 5% of wetting agent and the balance of filler, wherein the pharmaceutical active ingredient comprises difenoconazole and triphenyltin acetate in a weight ratio of 10: 1; the dispersing agent is formed by mixing sodium naphthalene sulfonate and sodium lignosulfonate according to the mass ratio of 1.5: 1; the wetting agent is prepared by mixing sodium dodecyl sulfate and sodium lignosulphonate according to the mass ratio of 1.2: 1; the filler is 30% of white carbon black and 70% of talcum powder.
The bactericide composition containing the triphenyltin acetate and the difenoconazole is prepared by the following method: crushing the fillers in percentage by weight by using a crusher, and sieving the crushed fillers with a 325-mesh sieve; and (2) sequentially putting the filler, the dispersing agent, the wetting agent and the pharmaceutical active ingredients into a stirring container according to the mass percentage, stirring for 40 minutes, crushing the product, sieving by using a 30-55 nm sieve, crushing for 20 minutes by using a jet mill, cooling the product, detecting and packaging to obtain the finished product.
Example 5
Bactericide composition containing triphenyltin acetate and difenoconazole and preparation method thereof
The bactericide composition is in the form of dispersible oil suspending agent, takes an organic solvent as a medium, and comprises the following components in percentage by weight: 1-60% of active pharmaceutical ingredients, 0-20% of wetting agent, 0-20% of dispersing agent, 0.2-20% of emulsifying agent, 0-10% of suspending aid and the balance of dispersing medium, wherein the active pharmaceutical ingredients comprise difenoconazole and triphenyl tin acetate in a weight ratio of 1: 10; the wetting agent is sodium dodecyl sulfate; the emulsifier is formed by mixing calcium dodecyl benzene sulfonate and castor oil polyoxyethylene ether according to the ratio of 1: 0.5-2; the dispersing agent is formed by mixing an alkylphenol polyoxyethylene ether formaldehyde condensate and fatty alcohol polyoxyethylene ether sulfate according to the ratio of 10: 4-15; the suspension auxiliary agent is formed by mixing white carbon black and organic bentonite according to a ratio of 1: 1; the dispersion medium is methyl oleate.
The invention also aims to provide a preparation method of the bactericidal agent composition containing the triphenyltin acetate and the difenoconazole, which comprises the following steps: adding the pharmaceutical active ingredients, the wetting agent, the dispersing agent, the emulsifier, the suspension auxiliary agent and the dispersion medium in percentage into a feeding kettle, and stirring and shearing for 20-40 minutes to obtain a suspension; and sanding the suspension until the particle size is 4-5 mu m to obtain the bactericidal agent composition containing the triphenyltin acetate and the difenoconazole.
Example 6
Bactericide composition containing triphenyltin acetate and difenoconazole and preparation method thereof
The bactericide composition is in the form of dispersible oil suspending agent, takes an organic solvent as a medium, and comprises the following components in percentage by weight: 1% of a medicinal active ingredient, 2% of a dispersing agent, 8% of an emulsifying agent and the balance of a dispersing medium, wherein the medicinal active ingredient comprises difenoconazole and triphenyltin acetate in a weight ratio of 1: 5; the wetting agent is sodium dodecyl sulfate; the emulsifier is formed by mixing calcium dodecyl benzene sulfonate and castor oil polyoxyethylene ether according to the ratio of 1: 0.5; the dispersing agent is formed by mixing an alkylphenol polyoxyethylene ether formaldehyde condensate and fatty alcohol polyoxyethylene ether sulfate according to the ratio of 10: 4; the suspension auxiliary agent is formed by mixing white carbon black and organic bentonite according to a ratio of 1: 1; the dispersion medium is methyl oleate.
The preparation method of the bactericide composition containing the triphenyltin acetate and the difenoconazole comprises the following steps: adding the pharmaceutical active ingredients, the wetting agent, the dispersing agent, the emulsifier, the suspension auxiliary agent and the dispersion medium in percentage into a feeding kettle, and stirring and shearing for 20 minutes to obtain a suspension; and sanding the suspension until the particle size is 4-5 mu m to obtain the bactericidal agent composition containing the triphenyltin acetate and the difenoconazole.
Example 7
Bactericide composition containing triphenyltin acetate and difenoconazole and preparation method thereof
The bactericide composition is in the form of dispersible oil suspending agent, takes an organic solvent as a medium, and comprises the following components in percentage by weight: 60% of a medicinal active ingredient, 1% of a wetting agent, 8% of a dispersing agent, 20% of an emulsifying agent, 10% of a suspending aid and the balance of a dispersing medium, wherein the medicinal active ingredient comprises difenoconazole and triphenyltin acetate in a weight ratio of 1: 1; the wetting agent is sodium dodecyl sulfate; the emulsifier is formed by mixing calcium dodecyl benzene sulfonate and castor oil polyoxyethylene ether according to a ratio of 1: 2; the dispersing agent is formed by mixing an alkylphenol polyoxyethylene ether formaldehyde condensate and fatty alcohol polyoxyethylene ether sulfate according to the ratio of 10: 15; the suspension auxiliary agent is formed by mixing white carbon black and organic bentonite according to a ratio of 1: 1; the dispersion medium is methyl oleate.
The invention also aims to provide a preparation method of the bactericidal agent composition containing the triphenyltin acetate and the difenoconazole, which comprises the following steps: adding the pharmaceutical active ingredients, the wetting agent, the dispersing agent, the emulsifier, the suspension auxiliary agent and the dispersion medium in percentage into a feeding kettle, and stirring and shearing for 40 minutes to obtain a suspension; and sanding the suspension until the particle size is 4-5 mu m to obtain the bactericidal agent composition containing the triphenyltin acetate and the difenoconazole.
Example 8
Bactericide composition containing triphenyltin acetate and difenoconazole and preparation method thereof
The bactericide composition is in the form of dispersible oil suspending agent, takes an organic solvent as a medium, and comprises the following components in percentage by weight: 50% of a medicinal active ingredient, 20% of a wetting agent, 20% of a dispersing agent, 2% of an emulsifying agent, 5% of a suspending aid and the balance of a dispersing medium, wherein the medicinal active ingredient comprises difenoconazole and triphenyltin acetate in a weight ratio of 10: 1; the wetting agent is sodium dodecyl sulfate; the emulsifier is formed by mixing calcium dodecyl benzene sulfonate and castor oil polyoxyethylene ether according to the ratio of 1: 1; the dispersing agent is formed by mixing an alkylphenol polyoxyethylene ether formaldehyde condensate and fatty alcohol polyoxyethylene ether sulfate according to the ratio of 10: 10; the suspension auxiliary agent is formed by mixing white carbon black and organic bentonite according to a ratio of 1: 1; the dispersion medium is methyl oleate.
The invention also aims to provide a preparation method of the bactericidal agent composition containing the triphenyltin acetate and the difenoconazole, which comprises the following steps: adding the pharmaceutical active ingredients, the wetting agent, the dispersing agent, the emulsifier, the suspension auxiliary agent and the dispersion medium in percentage into a feeding kettle, and stirring and shearing for 30 minutes to obtain a suspension; and sanding the suspension until the particle size is 4-5 mu m to obtain the bactericidal agent composition containing the triphenyltin acetate and the difenoconazole.
Example 9
Bactericide composition containing triphenyltin acetate and difenoconazole and preparation method thereof
The bactericide composition is in the form of dispersible oil suspending agent, takes an organic solvent as a medium, and comprises the following components in percentage by weight: 20% of medicinal active ingredients, 5% of wetting agent, 0.2% of emulsifier, 1% of suspending aid, 2% of chitosan oligosaccharide, 0.6% of common andrographis herb extract, 1.5% of folium artemisiae argyi extract, 1.8% of cortex phellodendri extract, 0.2-1.2% of brassinolide and the balance of dispersion medium, wherein the medicinal active ingredients comprise difenoconazole and triphenyl tin acetate in a weight ratio of 1: 5; the wetting agent is sodium dodecyl sulfate; the emulsifier is formed by mixing calcium dodecyl benzene sulfonate and castor oil polyoxyethylene ether according to the ratio of 1: 0.5-2; the dispersing agent is formed by mixing an alkylphenol polyoxyethylene ether formaldehyde condensate and fatty alcohol polyoxyethylene ether sulfate according to the ratio of 10: 4-15; the suspension auxiliary agent is formed by mixing white carbon black and organic bentonite according to a ratio of 1: 1; the dispersion medium is methyl oleate.
The invention also aims to provide a preparation method of the bactericidal agent composition containing the triphenyltin acetate and the difenoconazole, which comprises the following steps: adding the pharmaceutical active ingredients, the wetting agent, the dispersing agent, the emulsifier, the suspension auxiliary agent and the dispersion medium in percentage into a feeding kettle, and stirring and shearing for 30 minutes to obtain a suspension; and sanding the suspension until the particle size is 4-5 mu m to obtain the bactericidal agent composition containing the triphenyltin acetate and the difenoconazole.
Example 10
Bactericide composition containing triphenyltin acetate and difenoconazole and preparation method thereof
The bactericide composition is in the form of dispersible oil suspending agent, takes an organic solvent as a medium, and comprises the following components in percentage by weight: 20% of medicinal active ingredients, 5% of wetting agent, 8% of dispersing agent, 10% of emulsifying agent, 2% of suspending aid, 1.2% of chitosan oligosaccharide, 0.4% of andrographis paniculata extract, 0.2% of folium artemisiae argyi extract, 0.4% of cortex phellodendri extract, 0.2% of brassinolide and the balance of dispersing medium, wherein the medicinal active ingredients comprise difenoconazole and triphenyl tin acetate in a weight ratio of 1: 5; the wetting agent is sodium dodecyl sulfate; the emulsifier is formed by mixing calcium dodecyl benzene sulfonate and castor oil polyoxyethylene ether according to the ratio of 1: 1; the dispersing agent is formed by mixing an alkylphenol polyoxyethylene ether formaldehyde condensation compound and fatty alcohol polyoxyethylene ether sulfate according to the ratio of 1: 1; the suspension auxiliary agent is formed by mixing white carbon black and organic bentonite according to a ratio of 1: 1; the dispersion medium is methyl oleate.
The invention also aims to provide a preparation method of the bactericidal agent composition containing the triphenyltin acetate and the difenoconazole, which comprises the following steps: adding the pharmaceutical active ingredients, the wetting agent, the dispersing agent, the emulsifier, the suspension auxiliary agent and the dispersion medium in percentage into a feeding kettle, and stirring and shearing for 30 minutes to obtain a suspension; and sanding the suspension until the particle size is 4-5 mu m to obtain the bactericidal agent composition containing the triphenyltin acetate and the difenoconazole.
Example 11
Bactericide composition containing triphenyltin acetate and difenoconazole and preparation method thereof
The bactericide composition is in the form of dispersible oil suspending agent, takes an organic solvent as a medium, and comprises the following components in percentage by weight: 20% of a medicinal active ingredient, 5% of a wetting agent, 8% of a dispersing agent, 10% of an emulsifying agent, 2% of a suspending aid and the balance of a dispersing medium, wherein the medicinal active ingredient comprises difenoconazole and triphenyltin acetate in a weight ratio of 1: 10; the wetting agent is sodium dodecyl sulfate; the emulsifier is formed by mixing calcium dodecyl benzene sulfonate and castor oil polyoxyethylene ether according to the ratio of 1: 1; the dispersing agent is formed by mixing an alkylphenol polyoxyethylene ether formaldehyde condensation compound and fatty alcohol polyoxyethylene ether sulfate according to the ratio of 1: 1; the suspension auxiliary agent is formed by mixing white carbon black and organic bentonite according to a ratio of 1: 1; the dispersion medium is methyl oleate.
The invention also aims to provide a preparation method of the bactericidal agent composition containing the triphenyltin acetate and the difenoconazole, which comprises the following steps: adding the pharmaceutical active ingredients, the wetting agent, the dispersing agent, the emulsifier, the suspension auxiliary agent and the dispersion medium in percentage into a feeding kettle, and stirring and shearing for 30 minutes to obtain a suspension; and sanding the suspension until the particle size is 4-5 mu m to obtain the bactericidal agent composition containing the triphenyltin acetate and the difenoconazole.
Example 12
Bactericide composition containing triphenyltin acetate and difenoconazole and preparation method thereof
The bactericide composition is in the form of dispersible oil suspending agent, takes an organic solvent as a medium, and comprises the following components in percentage by weight: 20% of a medicinal active ingredient, 5% of a wetting agent, 8% of a dispersing agent, 10% of an emulsifying agent, 2% of a suspension aid and the balance of a dispersing medium, wherein the medicinal active ingredient comprises difenoconazole and triphenyltin acetate in a weight ratio of 1: 5; the wetting agent is sodium dodecyl sulfate; the emulsifier is formed by mixing calcium dodecyl benzene sulfonate and castor oil polyoxyethylene ether according to the ratio of 1: 1; the dispersing agent is formed by mixing an alkylphenol polyoxyethylene ether formaldehyde condensation compound and fatty alcohol polyoxyethylene ether sulfate according to the ratio of 1: 1; the suspension auxiliary agent is formed by mixing white carbon black and organic bentonite according to a ratio of 1: 1; the dispersion medium is methyl oleate.
The preparation method is the same as example 11.
Example 13
Bactericide composition containing triphenyltin acetate and difenoconazole and preparation method thereof
The bactericide composition is in the form of dispersible oil suspending agent, takes an organic solvent as a medium, and comprises the following components in percentage by weight: 20% of a medicinal active ingredient, 5% of a wetting agent, 8% of a dispersing agent, 10% of an emulsifying agent, 2% of a suspension aid and the balance of a dispersion medium, wherein the medicinal active ingredient comprises difenoconazole and triphenyltin acetate in a weight ratio of 1: 1; the wetting agent is sodium dodecyl sulfate; the emulsifier is formed by mixing calcium dodecyl benzene sulfonate and castor oil polyoxyethylene ether according to the ratio of 1: 1; the dispersing agent is formed by mixing an alkylphenol polyoxyethylene ether formaldehyde condensation compound and fatty alcohol polyoxyethylene ether sulfate according to the ratio of 1: 1; the suspension auxiliary agent is formed by mixing white carbon black and organic bentonite according to a ratio of 1: 1; the dispersion medium is methyl oleate.
The preparation method is the same as example 11.
Example 14
Bactericide composition containing triphenyltin acetate and difenoconazole and preparation method thereof
The bactericide composition is in the form of dispersible oil suspending agent, takes an organic solvent as a medium, and comprises the following components in percentage by weight: 20% of a medicinal active ingredient, 5% of a wetting agent, 8% of a dispersing agent, 10% of an emulsifying agent, 2% of a suspending aid and the balance of a dispersing medium, wherein the medicinal active ingredient comprises difenoconazole and triphenyltin acetate in a weight ratio of 10: 1; the wetting agent is sodium dodecyl sulfate; the emulsifier is formed by mixing calcium dodecyl benzene sulfonate and castor oil polyoxyethylene ether according to the ratio of 1: 1; the dispersing agent is formed by mixing an alkylphenol polyoxyethylene ether formaldehyde condensation compound and fatty alcohol polyoxyethylene ether sulfate according to the ratio of 1: 1; the suspension auxiliary agent is formed by mixing white carbon black and organic bentonite according to a ratio of 1: 1; the dispersion medium is methyl oleate.
The preparation method is the same as example 11.
Example 15
Bactericide composition containing triphenyltin acetate and difenoconazole and preparation method thereof
The bactericide composition is in the form of dispersible oil suspending agent, takes an organic solvent as a medium, and comprises the following components in percentage by weight: 1% of a medicinal active ingredient, 5% of a wetting agent, 8% of a dispersing agent, 10% of an emulsifying agent, 2% of a suspension aid and the balance of a dispersion medium, wherein the medicinal active ingredient comprises difenoconazole and triphenyltin acetate in a weight ratio of 5: 1; the wetting agent is sodium dodecyl sulfate; the emulsifier is formed by mixing calcium dodecyl benzene sulfonate and castor oil polyoxyethylene ether according to the ratio of 1: 1; the dispersing agent is formed by mixing an alkylphenol polyoxyethylene ether formaldehyde condensation compound and fatty alcohol polyoxyethylene ether sulfate according to the ratio of 1: 1; the suspension auxiliary agent is formed by mixing white carbon black and organic bentonite according to a ratio of 1: 1; the dispersion medium is methyl oleate.
The preparation method is the same as example 11.
Example 16
Bactericide composition containing triphenyltin acetate and difenoconazole and preparation method thereof
The bactericide composition is in the form of dispersible oil suspending agent, takes an organic solvent as a medium, and comprises the following components in percentage by weight: the suspension concentrate comprises 10% of a medicinal active ingredient, 5% of a wetting agent, 8% of a dispersing agent, 10% of an emulsifying agent, 2% of a suspension aid and the balance of a dispersing medium, wherein the medicinal active ingredient comprises difenoconazole and triphenyltin acetate in a weight ratio of 1: 5; the wetting agent is sodium dodecyl sulfate; the emulsifier is formed by mixing calcium dodecyl benzene sulfonate and castor oil polyoxyethylene ether according to the ratio of 1: 1; the dispersing agent is formed by mixing an alkylphenol polyoxyethylene ether formaldehyde condensation compound and fatty alcohol polyoxyethylene ether sulfate according to the ratio of 1: 1; the suspension auxiliary agent is formed by mixing white carbon black and organic bentonite according to a ratio of 1: 1; the dispersion medium is methyl oleate.
The preparation method is the same as example 11.
Example 17
Bactericide composition containing triphenyltin acetate and difenoconazole and preparation method thereof
The bactericide composition is in the form of dispersible oil suspending agent, takes an organic solvent as a medium, and comprises the following components in percentage by weight: 50% of a medicinal active ingredient, 5% of a wetting agent, 8% of a dispersing agent, 10% of an emulsifying agent, 2% of a suspending aid and the balance of a dispersing medium, wherein the medicinal active ingredient comprises difenoconazole and triphenyltin acetate in a weight ratio of 1: 5; the wetting agent is sodium dodecyl sulfate; the emulsifier is formed by mixing calcium dodecyl benzene sulfonate and castor oil polyoxyethylene ether according to the ratio of 1: 1; the dispersing agent is formed by mixing an alkylphenol polyoxyethylene ether formaldehyde condensation compound and fatty alcohol polyoxyethylene ether sulfate according to the ratio of 1: 1; the suspension auxiliary agent is formed by mixing white carbon black and organic bentonite according to a ratio of 1: 1; the dispersion medium is methyl oleate.
The preparation method is the same as example 11.
Example 18
Bactericide composition containing triphenyltin acetate and difenoconazole and preparation method thereof
The bactericide composition is in the form of dispersible oil suspending agent, takes an organic solvent as a medium, and comprises the following components in percentage by weight: 70% of medicinal active ingredients, 5% of wetting agent, 8% of dispersing agent, 10% of emulsifying agent, 2% of suspending aid and the balance of dispersing medium, wherein the medicinal active ingredients comprise difenoconazole and triphenyltin acetate in a weight ratio of 1: 5; the wetting agent is sodium dodecyl sulfate; the emulsifier is formed by mixing calcium dodecyl benzene sulfonate and castor oil polyoxyethylene ether according to the ratio of 1: 1; the dispersing agent is formed by mixing an alkylphenol polyoxyethylene ether formaldehyde condensation compound and fatty alcohol polyoxyethylene ether sulfate according to the ratio of 1: 1; the suspension auxiliary agent is formed by mixing white carbon black and organic bentonite according to a ratio of 1: 1; the dispersion medium is methyl oleate.
The preparation method is the same as example 11.
Example 19
Bactericide composition containing triphenyltin acetate and difenoconazole and preparation method thereof
The bactericide composition is in the form of dispersible oil suspending agent, takes an organic solvent as a medium, and comprises the following components in percentage by weight: 1% of medicinal active ingredients, 5% of wetting agent, 8% of dispersing agent, 10% of emulsifying agent, 2% of suspending aid, 3.2% of chitosan oligosaccharide, 1.2% of andrographis paniculata extract, 2.5% of folium artemisiae argyi extract, 1.6% of cortex phellodendri extract, 1.2% of brassinolide and the balance of dispersing medium, wherein the medicinal active ingredients comprise difenoconazole and triphenyl tin acetate in a weight ratio of 1: 5; the wetting agent is sodium dodecyl sulfate; the emulsifier is formed by mixing calcium dodecyl benzene sulfonate and castor oil polyoxyethylene ether according to the ratio of 1: 1; the dispersing agent is formed by mixing an alkylphenol polyoxyethylene ether formaldehyde condensation compound and fatty alcohol polyoxyethylene ether sulfate according to the ratio of 1: 1; the suspension auxiliary agent is formed by mixing white carbon black and organic bentonite according to a ratio of 1: 1; the dispersion medium is methyl oleate.
The preparation method is the same as example 11.
Example 20
Bactericide composition containing triphenyltin acetate and difenoconazole and preparation method thereof
The bactericide composition is in the form of dispersible oil suspending agent, takes an organic solvent as a medium, and comprises the following components in percentage by weight: 60% of medicinal active ingredients, 5% of wetting agent, 8% of dispersing agent, 10% of emulsifying agent, 2% of suspending aid, 3.2% of chitosan oligosaccharide, 1.2% of andrographis paniculata extract, 2.5% of folium artemisiae argyi extract, 1.6% of cortex phellodendri extract, 1.2% of brassinolide and the balance of dispersing medium, wherein the medicinal active ingredients comprise difenoconazole and triphenyl tin acetate in a weight ratio of 1: 5; the wetting agent is sodium dodecyl sulfate; the emulsifier is formed by mixing calcium dodecyl benzene sulfonate and castor oil polyoxyethylene ether according to the ratio of 1: 1; the dispersing agent is formed by mixing an alkylphenol polyoxyethylene ether formaldehyde condensation compound and fatty alcohol polyoxyethylene ether sulfate according to the ratio of 1: 1; the suspension auxiliary agent is formed by mixing white carbon black and organic bentonite according to a ratio of 1: 1; the dispersion medium is methyl oleate.
The preparation method is the same as example 11.
Comparative example 1
Bactericide composition and preparation method thereof
The bactericide composition is in the form of dispersible oil suspending agent, takes an organic solvent as a medium, and comprises the following components in percentage by weight: 20% of a medicinal active ingredient, 5% of a wetting agent, 8% of a dispersing agent, 10% of an emulsifying agent, 2% of a suspension aid and the balance of a dispersion medium, wherein the medicinal active ingredient is difenoconazole; the wetting agent is sodium dodecyl sulfate; the emulsifier is formed by mixing calcium dodecyl benzene sulfonate and castor oil polyoxyethylene ether according to the ratio of 1: 1; the dispersing agent is formed by mixing an alkylphenol polyoxyethylene ether formaldehyde condensation compound and fatty alcohol polyoxyethylene ether sulfate according to the ratio of 1: 1; the suspension auxiliary agent is formed by mixing white carbon black and organic bentonite according to a ratio of 1: 1; the dispersion medium is methyl oleate.
The preparation method is the same as example 11.
Comparative example 2
Bactericide composition and preparation method thereof
The bactericide composition is in the form of dispersible oil suspending agent, takes an organic solvent as a medium, and comprises the following components in percentage by weight: 20% of a medicinal active ingredient, 5% of a wetting agent, 8% of a dispersing agent, 10% of an emulsifying agent, 2% of a suspension aid and the balance of a dispersion medium, wherein the medicinal active ingredient is triphenyl tin acetate; the wetting agent is sodium dodecyl sulfate; the emulsifier is formed by mixing calcium dodecyl benzene sulfonate and castor oil polyoxyethylene ether according to the ratio of 1: 1; the dispersing agent is formed by mixing an alkylphenol polyoxyethylene ether formaldehyde condensation compound and fatty alcohol polyoxyethylene ether sulfate according to the ratio of 1: 1; the suspension auxiliary agent is formed by mixing white carbon black and organic bentonite according to a ratio of 1: 1; the dispersion medium is methyl oleate.
The preparation method is the same as example 11.
Examples of the experiments
To further illustrate the technological advancement of the present invention, experiments are now taken to further illustrate it.
1. Determination of the Cotoxicity coefficient
50g of a mixture M of difenoconazole and triphenyltin acetate were prepared as described in examples 11 to 141、M2、M3、M4The difenoconazole is used as a standard single agent, 50g of triphenyltin acetate is used as a standard single agent, the toxicity index is K, and the percentage content is P.
Preparing a sample A from difenoconazole raw medicine acetone and a sample B from triphenyltin acetate on a superclean workbench, and preparing a mixed agent M1、M2、M3、M4Adding a sterilized culture dish into each sample conical flask, introducing downy mildew suspension as a strain, culturing for 5 days under constant-temperature dark conditions, and testing the bacteriostasis percentage of each sample.
Measuring the toxicity regression equation of the mixture, difenoconazole and triphenyltin acetate by a conventional method to obtain LC50. The actual toxicity index and the theoretical toxicity index of the fungicide composition containing the triphenyltin acetate and the difenoconazole prepared in the embodiments 11 to 14 are calculated by taking the difenoconazole as a standard medicament. The co-toxicity coefficient (CTC) was calculated and the results are shown in table 1.
The calculation method comprises the following steps: the fungicide composition containing triphenyltin acetate and difenoconazole prepared in examples 11 to 14 was M1、M2、M3、M4The difenoconazole is A, the triphenyltin acetate is B, the toxicity index is K, the percentage content is P, and the difenoconazole is used as a standard single agent.
Virulence index K of difenoconazoleAComprises the following steps: LC of [ Difenoconazole50LC of difenoconazole50]×100＝100；
Virulence index K of triphenyltin acetateBComprises the following steps: LC of [ Difenoconazole50LC of/Triphenyl tin acetate50]×100；
Actual virulence index K of MMComprises the following steps: LC of [ Difenoconazole50LC of/M50]×100；
Theoretical virulence index K of MMComprises the following steps: kA×PA+KB×PB
Co-toxicity coefficient (CTC) is: [ actual virulence index of M/theoretical virulence index of M ]. times.100
TABLE 1 virulence determination results for single prodrugs and mixtures
LC50(mg/mL)
Measured virulence index
Theoretical virulence index
Co-toxicity coefficient
Difenoconazole (A)
1.205
100
-
-
Triphenyltin acetate (B)
13.826
8.715
-
-
A:B＝1:10
5.485
1.205
13.826
129.123
A:B＝1:5
3.561
1.205
13.826
141.410
A:B＝1:1
1.024
1.205
13.826
216.484
A:B＝10:1
1.053
1.205
13.826
124.791
2. The product performance of the dispersible oil suspending agent containing the triphenyltin acetate and difenoconazole bactericide composition is determined, and the result is shown in table 2.
Table 2 Performance test results of the fungicide compositions prepared in examples 5 to 20 of the present invention
3. Field test
Drug effect test for preventing and controlling wheat sharp eyespot in field test
The test is arranged to be carried out in wheat fields in the new countryside city in Henan, and 2 treatments are respectively set as follows: treatment 1: spraying clear water, and blank control; and (3) treatment 2: the bactericide compositions obtained in examples 11 to 15 and comparative example.
Wherein, the bactericide compositions obtained in examples 11 to 15 and comparative example were subjected to spray treatment of stem leaves at an active ingredient dose of 480 g/ha.
Spraying the composition once every 7 days for 2 times at the initial stage of wheat stripe blight. For the experiments, 6 parallel experimental zones were selected, each zone being dosed according to table 3. The application method comprises the following steps: the dosage of the preparation required in the embodiment of each test area is calculated according to the dosage of the active ingredients, the preparation is uniformly sprayed on the test area in a manual mode (the application water dosage per hectare is 480kg), and the control preparation is applied in the same mode. The medicine is applied in the morning with a sunny day, the highest temperature of 26 ℃ and the lowest temperature of 12 ℃. Meanwhile, 1 area is selected as a blank control area, and no medicine is sprayed.
20 plants were sampled and investigated at 5 points per plot by the control line method, 4 leaves were investigated for each plant, and the total leaf number and the number of diseased leaves at each stage were recorded.
The grading method comprises the following steps:
level 0: no disease;
level 1: the area of the lesion spots accounts for less than 5% of the area of the whole leaf;
and 3, level: the area of the lesion spots accounts for 6 to 25 percent of the area of the whole leaf;
and 5, stage: the area of the lesion spots accounts for 26-50% of the area of the whole leaf;
and 7, stage: the area of the lesion spots accounts for 51-75% of the area of the whole leaf;
and 9, stage: the area of the lesion spots accounts for more than 75 percent of the area of the whole leaf;
investigation time and number of times:
the disease condition base is investigated before the application of the medicine, and the prevention and treatment effect is investigated 7 days after the last application of the medicine.
The drug effect calculation method comprises the following steps:
the experimental results are shown below:
TABLE 3 efficacy test of the fungicide composition for controlling wheat stripe blight
The above is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and various modifications and changes will occur to those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
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