阅读说明：本技术 一种含三苯基乙酸锡与丙环唑的杀菌组合物及其制备方法 (Bactericidal composition containing triphenyltin acetate and propiconazole 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：本发明公开了一种含三苯基乙酸锡与丙环唑的杀菌组合物及其制备方法,所述杀菌组合物以三苯基乙酸锡与丙环唑为主要活性成分,其中三苯基乙酸锡与丙环唑重量比为1:10～10:1。该杀菌组合物将三苯基乙酸锡与丙环唑复配使用,具有较高的的协同增效杀菌作用,本发明杀菌组合物扩大了杀菌防治谱,提高了杀菌效率,避免了病害的抗药性,延长了药物持效期,克服了病菌的抗药性。本发明杀菌组合物可应用于蔬菜、果树病害上的防治,特别是在防治蔬菜、果树黑星病、斑点落叶病、晚疫病、纹枯病、赤霉等病害中有显著的杀菌防治效果,效果明显优于单剂使用防治效果。(The invention discloses a bactericidal composition containing triphenyltin acetate and propiconazole and a preparation method thereof, wherein the bactericidal composition takes the triphenyltin acetate and the propiconazole as main active ingredients, and the weight ratio of the triphenyltin acetate to the propiconazole is 1: 10-10: 1. The bactericidal composition combines the triphenyltin acetate and the propiconazole for use, has higher synergistic bactericidal action, expands the bactericidal control spectrum, improves the bactericidal efficiency, avoids the drug resistance of diseases, prolongs the drug duration and overcomes the drug resistance of germs. The bactericidal composition can be applied to the prevention and treatment of diseases of vegetables and fruit trees, particularly has obvious bactericidal prevention and treatment effects in the prevention and treatment of diseases of vegetables and fruit trees, scab, alternaria leaf spot, late blight, gibberellic disease and the like, and the effect is obviously superior to the prevention and treatment effect of single agent use.)

1. The bactericidal composition containing the triphenyltin acetate and the propiconazole is characterized in that active ingredients of the bactericidal composition are the triphenyltin acetate and the propiconazole, wherein the weight ratio of the triphenyltin acetate to the propiconazole is 1: 10-10: 1.

2. The bactericidal composition containing triphenyltin acetate and propiconazole according to claim 1, wherein the active ingredients of the bactericidal composition are triphenyltin acetate and propiconazole, and the weight ratio of the triphenyltin acetate to the propiconazole is 1: 1-5: 1.

3. The bactericidal composition containing triphenyltin acetate and propiconazole according to claim 1, wherein the dosage form of the bactericidal composition containing triphenyltin acetate and propiconazole is wettable powder or dispersible oil suspension.

4. The bactericidal composition containing the triphenyltin acetate and the propiconazole according to any one of claims 1 to 3, wherein the dosage form of the bactericidal composition is wettable powder and comprises the following components in percentage by weight: 1-80% of triphenyltin acetate and propiconazole, 1-10% of dispersing agent, 1-10% of wetting agent and the balance of filler;

the dispersing agent is formed by mixing sodium naphthalene sulfonate and calcium lignosulfonate according to the mass ratio of 1-2: 1; the wetting agent is formed by mixing sodium dodecyl sulfate and sodium lignin sulfonate according to the mass ratio of 1: 0.5-1.5; the filler is formed by mixing 20% of white carbon black and 80% of diatomite.

5. The bactericidal composition containing triphenyltin acetate and propiconazole according to claim 4, wherein the dosage form of the bactericidal composition is wettable powder, and the bactericidal composition is prepared by the following steps: stirring and mixing the triphenyltin acetate and the propiconazole uniformly according to the weight percentage, adding the filler according to the weight percentage, adsorbing and mixing, then adding the dispersant and the wetting agent according to the weight percentage, uniformly mixing, spray drying, wherein the moisture content is lower than 5%, and performing jet milling and sieving with a 400-mesh sieve to obtain the wettable powder of the bactericidal composition containing the triphenyltin acetate and the propiconazole.

6. The bactericidal composition containing the triphenyltin acetate and the propiconazole according to any one of claims 1 to 3, wherein the bactericidal composition is in the form of a dispersed oil suspending agent, takes an organic solvent as a medium, and comprises the following components in percentage by weight: 20-50% of triphenyltin acetate and propiconazole, 2-8% of dispersing agent, 1-5% of wetting agent, 2-8% of emulsifying agent, 1-5% of suspension auxiliary agent and the balance of dispersing medium;

the dispersing agent is formed by mixing an alkylphenol polyoxyethylene ether formaldehyde condensate and fatty alcohol polyoxyethylene ether sulfate according to the mass ratio of 1: 1-2.5; the wetting agent is fatty alcohol polyoxyethylene; the emulsifier is formed by mixing benzyl phenol polyoxyethylene and castor oil polyoxyethylene ether according to the mass ratio of 1-1.5: 1; the suspension auxiliary agent is formed by mixing white carbon black and organic bentonite according to the mass ratio of 1: 0.5-1; the dispersion medium is methyl oleate; the antifreeze agent is glycerol.

7. The bactericidal composition containing triphenyltin acetate and propiconazole according to claim 6, wherein the bactericidal composition is in the form of a dispersed oil suspending agent and is prepared by the following steps: and stirring and mixing the triphenyltin acetate, the propiconazole, the dispersant, the wetting agent, the dispersion medium, the defoamer and the antifreeze agent uniformly in percentage by weight, pre-dispersing to form uniform slurry, sanding in a sand mill, homogenizing and emulsifying with the emulsifier in percentage by weight after the particle size reaches the requirement, stirring for 20-50 min in a high-speed shearing machine, and sampling to determine that the particle size reaches the requirement to obtain the bactericidal composition dispersed oil suspending agent containing the triphenyltin acetate and the propiconazole.

8. The bactericidal composition containing triphenyltin acetate and propiconazole according to claim 7, wherein the particle size is required to be less than 5 μm.

9. The application of the bactericidal composition containing the triphenyltin acetate and the propiconazole according to any one of claims 1 to 8 in controlling diseases of vegetables and fruit trees.

10. The use of the fungicidal composition containing triphenyltin acetate and propiconazole according to claim 9 for the control 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 compound pesticides, and particularly relates to a bactericidal composition containing triphenyltin acetate and propiconazole and a preparation method thereof.

Background

Propiconazole, chemical name: 1- [2-2, 4-dichlorophenyl) -4-propyl-1, 3-dioxolan-2-methyl ] -1 h-1, 2, 4-triazole, of formula: C15H17Cl2N3O 2. Propiconazole is a systemic triazole broad-spectrum bactericide with dual functions of protection and treatment, can be absorbed by roots, stems and leaves, can be quickly conducted upwards in plant bodies, prevents and treats diseases caused by ascomycetes, basidiomycetes and imperfect fungi, and has good vigorous seedling control effect on vegetables planted in a greenhouse in summer while preventing and treating the diseases. Propiconazole has the characteristics of wide bactericidal spectrum, high activity, high bactericidal speed, long persistent period, strong systemic conductivity and the like, is an important efficient bactericide for treating or spraying the surfaces of cash crops or seeds, and has better control effects on wheat take-all, powdery mildew, rust disease, root rot, rice bakanae disease and sigatoka.

Triphenyltin acetate, formula: C20H18O2Sn is a non-systemic bactericide which can be absorbed by root, stem and leaf, and has effect in inhibiting diseases caused by Phycomycetes and Oomycetes. Has better protection and treatment effects on bacterial diseases, can effectively prevent and treat some fungi which are sensitive to copper bactericides, and has better prevention effect on the brown spot of beet.

Along with the increasing difficulty of preventing and controlling plant germs, the enlargement of the planting area of crops, fruits, vegetables and the like, the enhancement of the antibacterial property of the plant germs to pesticides, the prevention and control effect of a single medicament is greatly reduced, and the prevention and control requirements of the plant germs are higher and higher. At present, the application of triphenyltin acetate and propiconazole in combination for 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 is not reported. Therefore, the bactericidal composition containing the triphenyltin acetate and the propiconazole is developed by combining and compounding the triphenyltin acetate and the propiconazole, has high-efficiency broad-spectrum bactericidal property, and has good effects of preventing and treating diseases such as powdery mildew, cladosporium cucumerinum, alternaria leaf spot and the like of crops.

Disclosure of Invention

The invention aims to provide the bactericidal composition containing the triphenyltin acetate and the propiconazole, which has the advantages of wide bactericidal spectrum, high bactericidal efficiency and long bactericidal persistence.

The invention also aims to provide a preparation method of the sterilization composition containing the triphenyl tin acetate and the propiconazole, and application of the sterilization composition in preparing medicines for 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 active ingredients of the sterilization composition are triphenyl tin acetate and propiconazole, wherein the weight ratio of the triphenyl tin acetate to the propiconazole is 1: 10-10: 1.

Preferably, the active ingredients of the bactericidal composition are triphenyltin acetate and propiconazole, wherein the weight ratio of the triphenyltin acetate to the propiconazole is 1: 1-5: 1.

Preferably, the dosage form of the bactericidal composition containing the triphenyltin acetate and the propiconazole is wettable powder or dispersible oil suspending agent.

Preferably, the dosage form of the bactericidal composition is wettable powder and consists of the following components in percentage by weight: 1-80% of triphenyltin acetate and propiconazole, 1-10% of dispersing agent, 1-10% of wetting agent and the balance of filler.

More preferably, the dispersing agent is formed by mixing sodium naphthalene sulfonate and calcium lignosulfonate according to the mass ratio of 1-2: 1; the wetting agent is formed by mixing sodium dodecyl sulfate and sodium lignin sulfonate according to the mass ratio of 1: 0.5-1.5; the filler is formed by mixing 20% of white carbon black and 80% of diatomite.

More preferably, the dosage form of the bactericidal composition is wettable powder and is prepared by the following steps: stirring and mixing the triphenyltin acetate and the propiconazole uniformly according to the weight percentage, adding the filler according to the weight percentage, adsorbing and mixing, then adding the dispersant and the wetting agent according to the weight percentage, uniformly mixing, spray drying, wherein the moisture content is lower than 5%, and performing jet milling and sieving with a 400-mesh sieve to obtain the wettable powder of the bactericidal composition containing the triphenyltin acetate and the propiconazole.

Preferably, the formulation of the bactericidal composition is a dispersed oil suspending agent, takes an organic solvent as a medium, and consists of the following components in percentage by weight: 20-50% of triphenyltin acetate and propiconazole, 2-8% of dispersing agent, 1-5% of wetting agent, 2-8% of emulsifying agent, 1-5% of suspension auxiliary agent and the balance of dispersing medium.

Preferably, the dispersing agent is formed by mixing an alkylphenol polyoxyethylene ether formaldehyde condensate and fatty alcohol polyoxyethylene ether sulfate according to the mass ratio of 1: 1-2.5; the wetting agent is fatty alcohol polyoxyethylene; the emulsifier is formed by mixing benzyl phenol polyoxyethylene and castor oil polyoxyethylene ether according to the mass ratio of 1-1.5: 1; the suspension auxiliary agent is formed by mixing white carbon black and organic bentonite according to the mass ratio of 1: 0.5-1; the dispersion medium is methyl oleate; the antifreeze agent is glycerol.

More preferably, the formulation of the bactericidal composition is a dispersed oil suspending agent, and the bactericidal composition is prepared by the following steps: and stirring and mixing the triphenyltin acetate, the propiconazole, the dispersant, the wetting agent, the dispersion medium, the defoamer and the antifreeze agent uniformly in percentage by weight, pre-dispersing to form uniform slurry, sanding in a sand mill, homogenizing and emulsifying with the emulsifier in percentage by weight after the particle size reaches the requirement, stirring for 20-50 min in a high-speed shearing machine, and sampling to determine that the particle size reaches the requirement to obtain the bactericidal composition dispersed oil suspending agent containing the triphenyltin acetate and the propiconazole.

More preferably, the particle size is required to be less than 5 microns.

Preferably, the bactericidal composition containing the triphenyltin acetate and the propiconazole is applied to controlling diseases of vegetables and fruit trees.

Preferably, the sterilization composition containing the triphenyltin acetate and the propiconazole 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.

According to the technical scheme, the invention has the beneficial effects that:

(1) the sterilization composition containing the triphenyltin acetate and the propiconazole, which is prepared by the invention, has an obvious synergistic effect when the triphenyltin acetate and the propiconazole are compounded, has an increased application range compared with a single medicament, and especially has an obvious synergistic effect on preventing and treating diseases such as scab, alternaria leaf spot, late blight, downy mildew, rust disease, powdery mildew, banded sclerotial blight, gibberellic disease and the like.

(2) The bactericidal composition wettable powder containing the triphenyltin acetate and the propiconazole, which is prepared by the invention, has high uniformity of all components, high storage stability and convenient use; the bactericidal composition containing the triphenyltin acetate and the propiconazole prepared by the invention has the advantages of obvious synergistic effect, high pesticide effect, good prevention and treatment effect, excellent dispersion in water during use, cloudiness dispersion, good heat storage stability, and no phenomena of agglomeration, bag expansion, layering, precipitation and the like after long-term storage.

(3) The sterilization composition preparation containing the triphenyltin acetate and the propiconazole prepared by the invention is stable and reliable, the production process is simple, the cost performance of the product is high, and the environmental pollution and the harm to the body of a user are reduced.

Detailed Description

In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to embodiments. The exemplary embodiments and descriptions of the present invention are provided to explain the present invention, but not to limit the present invention.

Example 1

Bactericidal composition containing triphenyltin acetate and propiconazole and preparation method thereof

The bactericidal composition wettable powder containing the triphenyltin acetate and the propiconazole comprises the following components in parts by mass: 1g of triphenyltin acetate, 10g of propiconazole, 1g of dispersing agent and 1g of wetting agent, and adding the filler to 100 g;

the dispersing agent is formed by mixing sodium naphthalene sulfonate and calcium lignosulfonate according to the mass ratio of 1: 1; the wetting agent is prepared by mixing sodium dodecyl sulfate and sodium lignosulphonate according to the mass ratio of 1: 0.5; the filler is prepared by mixing 20% of white carbon black and 80% of diatomite.

The wettable powder of the bactericidal composition containing the triphenyltin acetate and the propiconazole is prepared by the following steps: stirring and mixing the triphenyltin acetate and the propiconazole uniformly according to the mass, adding the filler with the mass, adsorbing and mixing, adding the dispersant and the wetting agent with the mass, uniformly mixing, spray-drying, wherein the moisture content is lower than 5%, and performing jet milling and sieving with a 400-mesh sieve to obtain the 11% wettable powder of the bactericidal composition of the triphenyltin acetate and the propiconazole.

Example 2

Bactericidal composition containing triphenyltin acetate and propiconazole and preparation method thereof

The bactericidal composition wettable powder containing the triphenyltin acetate and the propiconazole comprises the following components in parts by mass: 10g of triphenyltin acetate, 1g of propiconazole, 2g of dispersing agent and 2g of wetting agent, and adding the filler to 100 g;

the dispersing agent is formed by mixing sodium naphthalene sulfonate and calcium lignosulfonate according to the mass ratio of 1: 1; the wetting agent is prepared by mixing sodium dodecyl sulfate and sodium lignosulphonate according to the mass ratio of 1: 0.5; the filler is prepared by mixing 20% of white carbon black and 80% of diatomite.

The wettable powder of the bactericidal composition containing the triphenyltin acetate and the propiconazole is prepared by the following steps: stirring and mixing the triphenyltin acetate and the propiconazole uniformly according to the mass, adding the filler with the mass, adsorbing and mixing, adding the dispersant and the wetting agent with the mass, uniformly mixing, spray drying until the moisture content is lower than 5%, jet milling, and sieving with a 400-mesh sieve to obtain the bactericidal composition wettable powder of 11% of the triphenyltin acetate and the propiconazole

Example 3

Bactericidal composition containing triphenyltin acetate and propiconazole and preparation method thereof

The bactericidal composition wettable powder containing the triphenyltin acetate and the propiconazole comprises the following components in parts by mass: 10g of triphenyltin acetate, 20g of propiconazole, 3g of dispersing agent and 2g of wetting agent, wherein the filling material is added to 100 g;

the dispersing agent is formed by mixing sodium naphthalene sulfonate and calcium 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: 1; the filler is prepared by mixing 20% of white carbon black and 80% of diatomite.

The wettable powder of the bactericidal composition containing the triphenyltin acetate and the propiconazole is prepared by the following steps: stirring and mixing the triphenyltin acetate and the propiconazole uniformly according to the mass, adding the filler with the mass, adsorbing and mixing, adding the dispersant and the wetting agent with the mass, uniformly mixing, spray drying, and performing jet milling to obtain the 30% wettable powder of the bactericidal composition of the triphenyltin acetate and the propiconazole, wherein the moisture content is lower than 5%.

Example 4

Bactericidal composition containing triphenyltin acetate and propiconazole and preparation method thereof

The bactericidal composition wettable powder containing the triphenyltin acetate and the propiconazole comprises the following components in parts by mass: 5g of triphenyltin acetate, 25g of propiconazole, 2g of dispersing agent and 2g of wetting agent, wherein the filling material is added to 100 g;

the dispersing agent is formed by mixing sodium naphthalene sulfonate and calcium lignosulfonate according to the mass ratio of 1: 1; the wetting agent is prepared by mixing sodium dodecyl sulfate and sodium lignosulphonate according to the mass ratio of 1: 0.5; the filler is prepared by mixing 20% of white carbon black and 80% of diatomite.

The wettable powder of the bactericidal composition containing the triphenyltin acetate and the propiconazole is prepared by the following steps: stirring and mixing the triphenyltin acetate and the propiconazole uniformly according to the mass, adding the filler with the mass, adsorbing and mixing, adding the dispersant and the wetting agent with the mass, uniformly mixing, spray drying, and performing jet milling to obtain the 30% wettable powder of the bactericidal composition of the triphenyltin acetate and the propiconazole, wherein the moisture content is lower than 5%.

Example 5

Bactericidal composition of triphenyltin acetate and propiconazole and preparation method thereof

The bactericidal composition wettable powder containing the triphenyltin acetate and the propiconazole comprises the following components in parts by mass: 20g of triphenyltin acetate, 20g of propiconazole, 2g of dispersing agent and 2g of wetting agent, wherein the filling material is added to 100 g;

the dispersing agent is formed by mixing sodium naphthalene sulfonate and calcium lignosulfonate according to the mass ratio of 1: 1; the wetting agent is prepared by mixing sodium dodecyl sulfate and sodium lignosulphonate according to the mass ratio of 1: 0.5; the filler is prepared by mixing 20% of white carbon black and 80% of diatomite.

The wettable powder of the bactericidal composition containing the triphenyltin acetate and the propiconazole is prepared by the following steps: stirring and mixing the triphenyltin acetate and the propiconazole uniformly according to the mass, adding the filler with the mass, adsorbing and mixing, adding the dispersant and the wetting agent with the mass, uniformly mixing, spray drying until the moisture content is lower than 5%, jet milling, and sieving with a 400-mesh sieve to obtain the bactericidal composition wettable powder of 40% of the triphenyltin acetate and the propiconazole

Example 6

Bactericidal composition containing triphenyltin acetate and propiconazole and preparation method thereof

The bactericidal composition wettable powder containing the triphenyltin acetate and the propiconazole comprises the following components in parts by mass: 25g of triphenyltin acetate, 5g of propiconazole, 3g of dispersing agent and 5g of wetting agent, and adding the filler to 100 g;

the dispersing agent is formed by mixing sodium naphthalene sulfonate and calcium 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: 0.5; the filler is prepared by mixing 20% of white carbon black and 80% of diatomite.

The wettable powder of the bactericidal composition containing the triphenyltin acetate and the propiconazole is prepared by the following steps: stirring and mixing the triphenyltin acetate and the propiconazole uniformly according to the mass, adding the filler with the mass, adsorbing and mixing, adding the dispersant and the wetting agent with the mass, uniformly mixing, spray drying, and performing jet milling to obtain the 30% wettable powder of the bactericidal composition of the triphenyltin acetate and the propiconazole, wherein the moisture content is lower than 5%.

Example 7

Bactericidal composition containing triphenyltin acetate and propiconazole and preparation method thereof

The bactericidal composition wettable powder containing the triphenyltin acetate and the propiconazole comprises the following components in parts by mass: 6g of triphenyltin acetate, 36g of propiconazole, 2g of dispersing agent and 3g of wetting agent, and the filler is added to 100 g;

the dispersing agent is formed by mixing sodium naphthalene sulfonate and calcium lignosulfonate according to the mass ratio of 0.5: 1; the wetting agent is prepared by mixing sodium dodecyl sulfate and sodium lignosulphonate according to the mass ratio of 1: 0.5; the filler is prepared by mixing 20% of white carbon black and 80% of diatomite.

The wettable powder of the bactericidal composition containing the triphenyltin acetate and the propiconazole is prepared by the following steps: stirring and mixing the triphenyltin acetate and the propiconazole uniformly according to the mass, adding the filler with the mass, adsorbing and mixing, adding the dispersant and the wetting agent with the mass, uniformly mixing, spray-drying, wherein the moisture content is lower than 5%, and performing jet milling and sieving with a 400-mesh sieve to obtain the bactericidal composition wettable powder of 42% triphenyltin acetate and propiconazole.

Example 8

Bactericidal composition containing triphenyltin acetate and propiconazole and preparation method thereof

The bactericidal composition wettable powder containing the triphenyltin acetate and the propiconazole comprises the following components in parts by mass: 30g of triphenyltin acetate, 15gg of propiconazole, 3g of dispersing agent and 5g of wetting agent, wherein the amount of the filler is 100 g;

the dispersing agent is formed by mixing sodium naphthalene sulfonate and calcium lignosulfonate according to the mass ratio of 1: 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 prepared by mixing 20% of white carbon black and 80% of diatomite.

The wettable powder of the bactericidal composition containing the triphenyltin acetate and the propiconazole is prepared by the following steps: stirring and mixing the triphenyltin acetate and the propiconazole uniformly according to the mass, adding the filler with the mass, adsorbing and mixing, adding the dispersant and the wetting agent with the mass, uniformly mixing, spray-drying, wherein the moisture content is lower than 5%, and performing jet milling and sieving with a 400-mesh sieve to obtain the 45% wettable powder of the bactericidal composition of the triphenyltin acetate and the propiconazole.

Example 9

Bactericidal composition containing triphenyltin acetate and propiconazole and preparation method thereof

The bactericidal composition wettable powder containing the triphenyltin acetate and the propiconazole comprises the following components in parts by mass: 50g of triphenyltin acetate, 10g of propiconazole, 7g of dispersing agent and 6g of wetting agent, wherein the filling material is added to 100 g;

the dispersing agent is formed by mixing sodium naphthalene sulfonate and calcium 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: 1.5; the filler is prepared by mixing 20% of white carbon black and 80% of diatomite.

The wettable powder of the bactericidal composition containing the triphenyltin acetate and the propiconazole is prepared by the following steps: stirring and mixing the triphenyltin acetate and the propiconazole uniformly according to the mass, adding the filler with the mass, adsorbing and mixing, adding the dispersant and the wetting agent with the mass, uniformly mixing, spray-drying, wherein the moisture content is lower than 5%, and performing jet milling and sieving with a 400-mesh sieve to obtain the 60% wettable powder of the bactericidal composition of the triphenyltin acetate and the propiconazole.

Example 10

Bactericidal composition containing triphenyltin acetate and propiconazole and preparation method thereof

The bactericidal composition wettable powder containing the triphenyltin acetate and the propiconazole comprises the following components in parts by mass: 50g of triphenyltin acetate, 20g of propiconazole, 7g of dispersing agent and 7g of wetting agent, wherein the filling material is added to 100 g;

the dispersing agent is formed by mixing sodium naphthalene sulfonate and calcium lignosulfonate according to the mass ratio of 72: 1; the wetting agent is prepared by mixing sodium dodecyl sulfate and sodium lignin sulfonate according to the mass ratio of 1: 71; the filler is prepared by mixing 20% of white carbon black and 80% of diatomite.

The wettable powder of the bactericidal composition containing the triphenyltin acetate and the propiconazole is prepared by the following steps: stirring and mixing the triphenyltin acetate and the propiconazole uniformly according to the mass, adding the filler with the mass, adsorbing and mixing, adding the dispersant and the wetting agent with the mass, uniformly mixing, spray-drying, wherein the moisture content is lower than 5%, and performing jet milling and sieving with a 400-mesh sieve to obtain the bactericidal composition wettable powder of 70% of the triphenyltin acetate and the propiconazole.

Example 11

Bactericidal composition containing triphenyltin acetate and propiconazole and preparation method thereof

The bactericidal composition wettable powder containing the triphenyltin acetate and the propiconazole comprises the following components in parts by mass: 20g of triphenyltin acetate, 60g of propiconazole, 5g of dispersing agent and 4g of wetting agent, and adding the filler to 100 g;

the dispersing agent is formed by mixing sodium naphthalene sulfonate and calcium 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: 1.5; the filler is prepared by mixing 20% of white carbon black and 80% of diatomite.

The wettable powder of the bactericidal composition containing the triphenyltin acetate and the propiconazole is prepared by the following steps: stirring and mixing the triphenyltin acetate and the propiconazole uniformly according to the mass, adding the filler with the mass, adsorbing and mixing, adding the dispersant and the wetting agent with the mass, uniformly mixing, spray-drying, wherein the moisture content is lower than 5%, and performing jet milling and sieving with a 400-mesh sieve to obtain the 80% wettable powder of the bactericidal composition of the triphenyltin acetate and the propiconazole.

Example 12

Bactericidal composition containing triphenyltin acetate and propiconazole and preparation method thereof

The bactericidal composition dispersed oil suspending agent containing the triphenyltin acetate and the propiconazole takes an organic solvent as a medium and consists of the following components in parts by mass: 5g of triphenyltin acetate, 10g of propiconazole, 3g of dispersing agent, 2g of wetting agent, 2g of antifreeze agent, 2g of emulsifier, 1.5g of suspension auxiliary agent and 100g of dispersing medium;

the dispersing agent is formed by mixing an alkylphenol polyoxyethylene ether formaldehyde condensate and fatty alcohol polyoxyethylene ether sulfate according to the mass ratio of 1: 1.25; the wetting agent is fatty alcohol polyoxyethylene; the emulsifier is formed by mixing benzyl phenol polyoxyethylene and castor oil polyoxyethylene ether according to the mass ratio of 1: 1; the suspension auxiliary agent is formed by mixing white carbon black and organic bentonite according to the mass ratio of 1: 0.5; the dispersion medium is methoxy polyethylene glycol; the antifreeze is glycerol.

The bactericidal composition dispersed oil suspending agent containing the triphenyltin acetate and the propiconazole is prepared by the following steps: stirring and mixing the triphenyltin acetate, propiconazole, a dispersing agent, a wetting agent, a dispersing medium, a defoaming agent and an antifreeze agent uniformly, pre-dispersing to form uniform slurry, sanding in a sand mill, homogenizing and emulsifying with the emulsifier with the mass after the particle size is determined to be less than 5 micrometers, stirring for 20-50 min in a high-speed shearing machine, sampling and determining the particle size to be less than 5 micrometers, and thus obtaining the 15% triphenyltin acetate and propiconazole sterilization composition dispersed oil suspending agent.

Example 13

Bactericidal composition containing triphenyltin acetate and propiconazole and preparation method thereof

The bactericidal composition dispersed oil suspending agent containing the triphenyltin acetate and the propiconazole takes an organic solvent as a medium and consists of the following components in parts by mass: 10g of triphenyltin acetate, 10g of propiconazole, 2g of dispersing agent, 1g of wetting agent, 2g of antifreeze agent, 2g of emulsifier, 1g of suspension auxiliary agent and 100g of dispersing medium;

the dispersing agent is formed by mixing an alkylphenol polyoxyethylene ether formaldehyde condensate and fatty alcohol polyoxyethylene ether sulfate according to the mass ratio of 1: 1; the wetting agent is fatty alcohol polyoxyethylene; the emulsifier is formed by mixing benzyl phenol polyoxyethylene and castor oil polyoxyethylene ether according to the mass ratio of 1: 1; the suspension auxiliary agent is formed by mixing white carbon black and organic bentonite according to the mass ratio of 1: 0.5-1; the dispersion medium is methoxy polyethylene glycol; the antifreeze is glycerol.

The bactericidal composition dispersed oil suspending agent containing the triphenyltin acetate and the propiconazole is prepared by the following steps: stirring and mixing the triphenyltin acetate, propiconazole, a dispersing agent, a wetting agent, a dispersing medium, a defoaming agent and an antifreeze agent uniformly, pre-dispersing to form uniform slurry, sanding in a sand mill, homogenizing and emulsifying with the emulsifier with the mass after the particle size is determined to be less than 5 micrometers, stirring for 20-50 min in a high-speed shearing machine, sampling and determining the particle size to be less than 5 micrometers, and thus obtaining the 20% triphenyltin acetate and propiconazole sterilization composition dispersed oil suspending agent.

Example 14

Bactericidal composition containing triphenyltin acetate and propiconazole and preparation method thereof

The bactericidal composition dispersed oil suspending agent containing the triphenyltin acetate and the propiconazole takes an organic solvent as a medium and consists of the following components in parts by mass: 20g of triphenyltin acetate, 10g of propiconazole, 4g of dispersing agent, 3g of wetting agent, 3g of antifreeze agent, 2g of emulsifier, 2.5g of suspension auxiliary agent and 100g of dispersing medium;

the dispersing agent is formed by mixing an alkylphenol polyoxyethylene ether formaldehyde condensate and fatty alcohol polyoxyethylene ether sulfate according to the mass ratio of 1: 1; the wetting agent is fatty alcohol polyoxyethylene; the emulsifier is formed by mixing benzyl phenol polyoxyethylene and castor oil polyoxyethylene ether according to the mass ratio of 1: 1; the suspension auxiliary agent is formed by mixing white carbon black and organic bentonite according to the mass ratio of 1: 1; the dispersion medium is methoxy polyethylene glycol; the antifreeze is glycerol.

The bactericidal composition dispersed oil suspending agent containing the triphenyltin acetate and the propiconazole is prepared by the following steps: stirring and mixing the triphenyltin acetate, propiconazole, a dispersing agent, a wetting agent, a dispersing medium, a defoaming agent and an antifreeze agent uniformly, pre-dispersing to form uniform slurry, sanding in a sand mill, homogenizing and emulsifying with the emulsifier with the mass after the particle size is determined to be less than 5 micrometers, stirring for 20-50 min in a high-speed shearing machine, sampling and determining the particle size to be less than 5 micrometers, and thus obtaining the 30% triphenyltin acetate and propiconazole sterilization composition dispersed oil suspending agent.

Example 15

Bactericidal composition containing triphenyltin acetate and propiconazole and preparation method thereof

The bactericidal composition dispersed oil suspending agent containing the triphenyltin acetate and the propiconazole takes an organic solvent as a medium and consists of the following components in parts by mass: 5g of triphenyltin acetate, 25g of propiconazole, 3g of dispersant, 2g of wetting agent, 2g of antifreeze agent, 2g of emulsifier, 1g of suspension assistant and 100g of dispersion medium;

the dispersing agent is formed by mixing an alkylphenol polyoxyethylene ether formaldehyde condensate and fatty alcohol polyoxyethylene ether sulfate according to the mass ratio of 1: 1-2.5; the wetting agent is fatty alcohol polyoxyethylene; the emulsifier is prepared by mixing benzyl phenol polyoxyethylene and castor oil polyoxyethylene ether according to the mass ratio of 1-1.5: 1; the suspension auxiliary agent is formed by mixing white carbon black and organic bentonite according to the mass ratio of 1: 0.5-1; the dispersion medium is methoxy polyethylene glycol; the antifreeze is glycerol.

The bactericidal composition dispersed oil suspending agent containing the triphenyltin acetate and the propiconazole is prepared by the following steps: stirring and mixing the triphenyltin acetate, propiconazole, a dispersing agent, a wetting agent, a dispersing medium, a defoaming agent and an antifreeze agent uniformly, pre-dispersing to form uniform slurry, sanding in a sand mill, homogenizing and emulsifying with the emulsifier with the mass after the particle size is determined to be less than 5 micrometers, stirring for 20-50 min in a high-speed shearing machine, sampling and determining the particle size to be less than 5 micrometers, and thus obtaining the 30% triphenyltin acetate and propiconazole sterilization composition dispersed oil suspending agent.

Example 16

Bactericidal composition containing triphenyltin acetate and propiconazole and preparation method thereof

The bactericidal composition dispersed oil suspending agent containing the triphenyltin acetate and the propiconazole takes an organic solvent as a medium and consists of the following components in parts by mass: 25g of triphenyltin acetate, 5g of propiconazole, 3g of dispersing agent, 3g of wetting agent, 3g of antifreeze agent, 2g of emulsifier, 1g of suspension auxiliary agent and 100g of dispersing medium;

the dispersing agent is formed by mixing an alkylphenol polyoxyethylene ether formaldehyde condensate and fatty alcohol polyoxyethylene ether sulfate according to the mass ratio of 1: 1-2.5; the wetting agent is fatty alcohol polyoxyethylene; the emulsifier is prepared by mixing benzyl phenol polyoxyethylene and castor oil polyoxyethylene ether according to the mass ratio of 1-1.5: 1; the suspension auxiliary agent is formed by mixing white carbon black and organic bentonite according to the mass ratio of 1: 0.5-1; the dispersion medium is methoxy polyethylene glycol; the antifreeze is glycerol.

The bactericidal composition dispersed oil suspending agent containing the triphenyltin acetate and the propiconazole is prepared by the following steps: stirring and mixing the triphenyltin acetate, propiconazole, a dispersing agent, a wetting agent, a dispersing medium, a defoaming agent and an antifreeze agent uniformly, pre-dispersing to form uniform slurry, sanding in a sand mill, homogenizing and emulsifying with the emulsifier with the mass after the particle size is determined to be less than 5 micrometers, stirring for 20-50 min in a high-speed shearing machine, sampling and determining the particle size to be less than 5 micrometers, and thus obtaining the 30% triphenyltin acetate and propiconazole sterilization composition dispersed oil suspending agent.

Example 17

Bactericidal composition containing triphenyltin acetate and propiconazole and preparation method thereof

The bactericidal composition dispersed oil suspending agent containing the triphenyltin acetate and the propiconazole takes an organic solvent as a medium and consists of the following components in parts by mass: 40g of triphenyltin acetate, 5g of propiconazole, 5g of dispersing agent, 3.5g of wetting agent, 3g of antifreeze agent, 4g of emulsifier, 2g of suspension auxiliary agent and 100g of dispersing medium;

the dispersing agent is formed by mixing an alkylphenol polyoxyethylene ether formaldehyde condensate and fatty alcohol polyoxyethylene ether sulfate according to the mass ratio of 1: 5; the wetting agent is fatty alcohol polyoxyethylene; the emulsifier is formed by mixing benzyl phenol polyoxyethylene and castor oil polyoxyethylene ether according to the mass ratio of 1.2: 1; the suspension auxiliary agent is formed by mixing white carbon black and organic bentonite according to the mass ratio of 1: 0.8; the dispersion medium is methoxy polyethylene glycol; the antifreeze is glycerol.

The bactericidal composition dispersed oil suspending agent containing the triphenyltin acetate and the propiconazole is prepared by the following steps: stirring and mixing the triphenyltin acetate, propiconazole, a dispersing agent, a wetting agent, a dispersing medium, a defoaming agent and an antifreeze agent uniformly, pre-dispersing to form uniform slurry, sanding in a sand mill, homogenizing and emulsifying with the emulsifier with the mass after the particle size is determined to be less than 5 micrometers, stirring for 20-50 min in a high-speed shearing machine, sampling and determining the particle size to be less than 5 micrometers, and thus obtaining the 45% of bactericidal composition dispersed oil suspension of the triphenyltin acetate and the propiconazole.

Example 18

Bactericidal composition containing triphenyltin acetate and propiconazole and preparation method thereof

The bactericidal composition dispersed oil suspending agent containing the triphenyltin acetate and the propiconazole takes an organic solvent as a medium and consists of the following components in parts by mass: 25g of triphenyltin acetate, 25g of propiconazole, 6g of dispersing agent, 4g of wetting agent, 4g of antifreeze agent, 4g of emulsifier, 3g of suspension auxiliary agent and 100g of dispersing medium;

the dispersing agent is formed by mixing an alkylphenol polyoxyethylene ether formaldehyde condensate and fatty alcohol polyoxyethylene ether sulfate according to the mass ratio of 1: 1; the wetting agent is fatty alcohol polyoxyethylene; the emulsifier is formed by mixing benzyl phenol polyoxyethylene and castor oil polyoxyethylene ether according to the mass ratio of 1.5: 1; the suspension auxiliary agent is formed by mixing white carbon black and organic bentonite according to the mass ratio of 1: 1; the dispersion medium is methoxy polyethylene glycol; the antifreeze is glycerol.

The bactericidal composition dispersed oil suspending agent containing the triphenyltin acetate and the propiconazole is prepared by the following steps: stirring and mixing the triphenyltin acetate, propiconazole, a dispersing agent, a wetting agent, a dispersing medium, a defoaming agent and an antifreeze agent uniformly, pre-dispersing to form uniform slurry, sanding in a sand mill, homogenizing and emulsifying with the emulsifier with the mass after the particle size is determined to be less than 5 micrometers, stirring for 20-50 min in a high-speed shearing machine, sampling and determining the particle size to be less than 5 micrometers, and thus obtaining the 50% of bactericidal composition dispersed oil suspension of the triphenyltin acetate and the propiconazole.

Example 19

Bactericidal composition containing triphenyltin acetate and propiconazole and preparation method thereof

The bactericidal composition dispersed oil suspending agent containing the triphenyltin acetate and the propiconazole takes an organic solvent as a medium and consists of the following components in parts by mass: 30g of triphenyltin acetate, 10g of propiconazole, 5g of dispersing agent, 3g of wetting agent, 3g of antifreeze agent, 5g of emulsifier, 3g of suspension auxiliary agent and 100g of dispersing medium;

the dispersing agent is formed by mixing an alkylphenol polyoxyethylene ether formaldehyde condensate and fatty alcohol polyoxyethylene ether sulfate according to the mass ratio of 1: 2.5; the wetting agent is fatty alcohol polyoxyethylene; the emulsifier is formed by mixing benzyl phenol polyoxyethylene and castor oil polyoxyethylene ether according to the mass ratio of 1.5: 1; the suspension auxiliary agent is formed by mixing white carbon black and organic bentonite according to the mass ratio of 1: 1; the dispersion medium is methoxy polyethylene glycol; the antifreeze is glycerol.

The bactericidal composition dispersed oil suspending agent containing the triphenyltin acetate and the propiconazole is prepared by the following steps: stirring and mixing the triphenyltin acetate, propiconazole, a dispersing agent, a wetting agent, a dispersing medium, a defoaming agent and an antifreeze agent uniformly, pre-dispersing to form uniform slurry, sanding in a sand mill, homogenizing and emulsifying with the emulsifier with the mass after the particle size is determined to be less than 5 micrometers, stirring for 20-50 min in a high-speed shearing machine, sampling and determining the particle size to be less than 5 micrometers, and thus obtaining the 40% of bactericidal composition dispersed oil suspension of the triphenyltin acetate and the propiconazole.

Comparative example 1

In contrast to example 8, triphenyltin acetate was absent.

Comparative example 2

In contrast to example 16, propiconazole was absent.

Test examples

In order to determine the performance of the bactericidal composition containing the triphenyltin acetate and the propiconazole, the bactericidal compositions containing the triphenyltin acetate and the propiconazole prepared in examples 1 to 7 and the bactericidal compositions containing the triphenyltin acetate and the propiconazole prepared in comparative examples 1 and 2 were respectively subjected to performance tests:

1. indoor bioassay test for bactericidal composition containing triphenyltin acetate and propiconazole

The method is characterized in that wheat sharp eyespot is taken as a test strain indoors, and the inhibition medium concentration EC of different agents on the strain is determined by adopting a hypha growth rate method₅₀Calculating the co-toxicity coefficient (CTC) of the mixture by adopting a Sun Yunpei co-toxicity coefficient calculation method, and determining the synergy of the mixture, wherein the calculation method comprises the following steps:

(1) using a single dosage of the mixture as a standard medicament (EC is usually selected)₅₀Lower), perform the calculation

(2) Single dose virulence index (standard dose EC)₅₀Single agent EC₅₀×100

(3) Measured virulence index of mixed preparation is EC of standard single preparation₅₀EC of value/blend₅₀Value x 100

(4) The theoretical virulence index of the mixed preparation is the virulence index of the A preparation, the content of the A preparation in the mixed preparation, the virulence index of the B preparation and the content of the B preparation in the mixed preparation

(5) Co-toxicity coefficient (CTC) of mixed preparation is measured toxicity index/mixed preparation theory toxicity index x 100

Evaluating the value of the mixture according to the value of CTC, wherein the CTC is larger than 120 and indicates that the mixture has synergy, the CTC is smaller than 80 and indicates that the mixture has antagonism, and the CTC is between 80 and 120 and indicates that the mixture has additive effect, generally, the CTC of the mixture is more than 120 which is the basic requirement of pesticide compound development.

The propiconazole A is propiconazole, and the propiconazole B is triphenyl tin acetate; the propiconazole is used as a standard medicament.

The indoor bioassay results are shown in table 1:

TABLE 1 indoor bioassay results of different ratios of triphenyltin acetate and propiconazole for wheat sharp eyespot

	EC50(mg/mL)	Measured virulence index	Theoretical virulence index	Co-toxicity coefficient
					Propiconazole (A)	6.6895	100	-	-
Triphenyltin acetate (B)	22.2596	30.0522	-	-
					A:B＝1:1	7.0235	95.2445	65.0261	146.4712
A:B＝2:1	5.2364	127.7499	76.6841	166.5925
					A:B＝1:5	12.3158	54.3164	41.7102	130.2233
A:B＝1:2	9.6623	69.2330	69.2330	129.7273
					A:B＝1:10	14.5783	42.9411	36.4111	124.8992

2. Field test example 1: drug effect test for preventing and controlling wheat sharp eyespot in field test

According to the wheat sharp eyespot pharmacodynamic test criterion, a proper test field is selected, the test is carried out in a wheat field in New and rural cities in Henan, the field soil fertility is consistent, the wheat growth vigor is good, the wheat is planted in the test field all the year round, and the occurrence condition of the wheat in a laboratory is an initial stage.

3 treatments are set in the field efficacy test, which respectively comprise: treatment 1: spraying clear water, and blank control; and (3) treatment 2: the bactericidal compositions containing triphenyltin acetate and tebuconazole prepared in examples 6 and 21; and (3) treatment: the fungicides prepared in comparative examples 1 and 2; the test areas with the dilution of 800 times are randomly arranged, the treatment is repeated for three times each time, and the stem and leaf spraying treatment is carried out according to the effective component dosage of 480 g/hectare.

The investigation, calculation and statistical method comprises the following steps: spraying the composition once every 7 days for 2 times at the initial stage of wheat stripe blight. For the experiments, 15 parallel experimental areas were selected, each area being administered according to table 2. 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 450kg), 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 are sampled and investigated at 5 points by a per-cell line comparison method, 4 leaves are investigated on each plant, namely the upper leaf, the middle leaf and the lower leaf, the total leaf number and the leaf number of each stage of disease are recorded, and disease indexes are calculated respectively.

The grading method comprises the following steps:

level 0: no disease spots;

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:

wherein:

CK₀-disease index before application in the clear water control zone;

CK₁-disease index after application in the clear water control zone;

PT₀-pre-dose disease index in the agent treatment area;

PT₁-disease index after drug treatment area application.

The test results are shown in table 2:

TABLE 2

The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and various modifications and changes may be made to the embodiment of the present invention by those skilled in the art. Any modification, equivalent replacement, or improvement made without departing from the spirit and principle of the present invention shall fall within the protection scope of the present invention.