Fluorine-containing pesticide wettable powder and preparation method thereof

Abstract

The invention provides wettable powder of a fluorine-containing pesticide and a preparation method of the wettable powder. The wettable powder of the fluorine-containing pesticide is prepared from the following components in parts by weight: 20 to 90 parts of fluopyram, 10 to 80 parts of fluazinam, 10 to 80 parts of trifluoro-imidazole amide, 10 to 60 parts of a surfactant, 0.1 to 5 parts of a stabilizer, 0.5 to 20 parts of an emulsifier and the balance of water. The wettable powder of the fluorine-containing pesticide has the advantages that the utilization rate of the pesticide (the wettable powder of the fluorine-containing pesticide) is increased, the biological control effect on pests and pathogenic bacteria is remarkably improved, pesticide residues are reduced, environmental pollution is reduced, and the wettable powder of the fluorine-containing pesticide is safe to people and livestock and has potential market value.

Description

Technical Field

[0001] The invention belongs to the technical field of pesticide preparation, and in particular relates to a wettable powder of a fluorine-containing pesticide and a preparation method thereof. Background Art

[0002] Insecticides and fungicides, as important components of pesticides, play an indispensable role in ensuring the health of humans and animals, promoting grain production and efficiency, maintaining ecological balance, and the long-term stable development of human social production activities and natural ecosystems.

[0003] Fluazinam has preventive and therapeutic effects and is effective against a variety of crop diseases, especially downy mildew, downy mildew, blight and late blight of cruciferous crops, anthracnose and powdery mildew of Chinese cabbage, and is an important member of the fungicide market. Fluazinam is a highly efficient new nematicide and insecticide, which is very stable in organic acid, amino acid and water solvents, has systemic conduction and ovicidal effects, and can effectively prevent and control various lepidoptera and coleoptera pests, especially a variety of piercing-sucking mouthparts pests, and has a good insecticidal effect on some resistant pests such as rice leaf roller. However, none of the three have fully exerted their effectiveness.

[0004] At the same time, with the continuous development and progress of society, the continuous improvement of people's living standards, the quality requirements for pesticides, including the ecology of pesticides, and people's increasing attention to human health issues, especially food safety issues, have further promoted the development trend of low-toxic pesticides. Developing high-quality and high-efficiency new formulations, increasing the utilization rate of the agent (the wettable powder of the fluorine-containing pesticide of the present invention), and expanding the effective range of the agent (the wettable powder of the fluorine-containing pesticide of the present invention) are hot spots in modern pesticide research and development, and are also an important development direction.

[0005] In the practice of pesticide production, due to the certain limitations of the control spectrum of single-component pesticides, it is often impossible to kill multiple harmful organisms of crop diseases at the same time. For this reason, people adopt the pesticides for controlling different pests and diseases to be mixed together (i.e., mixed agents) to expand the killing range, achieve the effect of one spray and multiple preventions, and play the role of mixed synergistic effect. However, due to the different proportions, it is easy to cause antagonism between different agents (wettable powders of fluorine-containing pesticides of the present invention), and even cause the drug effect to be reduced. And the difficulty of mixing different dosage forms is large, such as the pH of the mixed is not suitable, which will cause uneven mixing, and the agglomeration of particles will affect the effect of the agent (wettable powder of fluorine-containing pesticides of the present invention). Therefore, compounding needs to optimize the agent (wettable powder of fluorine-containing pesticides of the present invention) ratio, dosage form compatibility, and emulsifier selection to achieve good compounding effect and expand the scope of use. In addition, the development of modern agriculture requires that the compounding of pesticides has high efficiency, is economical and practical, and is environmentally friendly and pollution-free, and is friendly to the ecological environment, and is more conducive to human production and life. Summary of the invention

[0006] The present invention provides a wettable powder of a fluorine-containing pesticide and a preparation method thereof, which can at least solve the technical problems that different pesticides (the wettable powder of the fluorine-containing pesticide of the present invention) are easily antagonistic due to different proportions of pesticides mixed together (i.e., mixtures), and even lead to reduced efficacy; and different dosage forms are difficult to mix, for example, the pH of the mixture is not suitable, which will cause uneven mixing, particle agglomeration and other technical problems that affect the effect of the agent (the wettable powder of the fluorine-containing pesticide of the present invention).

[0007] The technical solution provided by the present invention is as follows:

[0008] In one aspect, a wettable powder of a fluorine-containing pesticide is provided, wherein the wettable powder of the fluorine-containing pesticide comprises the following components in parts by weight:

[0009] 20-90 parts of fluopyram, 10-80 parts of fluazinam, 10-80 parts of triflurimidine, 10-60 parts of surfactant, 0.1-5 parts of stabilizer, 0.5-20 parts of emulsifier, and the rest is water.

[0010] In an optional embodiment, the wettable powder of the fluorine-containing pesticide comprises the following components in parts by weight: 20-70 parts of fluopyram, 10-50 parts of fluazinam, 10-50 parts of triflumilast, 10-40 parts of surfactant, 0.1-1 part of stabilizer, 0.5-10 parts of emulsifier, and the rest is water.

[0011] In an optional embodiment, the surfactant includes one or more of naphthalenesulfonate, woodsulfonate, alkylsulfonate, aminosulfonate, fatty alcohol salt, polyoxyethylene alkyl ether, modified naphthalenesulfonate, modified woodsulfonate, and modified aminosulfonate.

[0012] In an optional embodiment, the stabilizer includes one or more of pentaerythritol, an antioxidant and creatinine.

[0013] In an optional embodiment, the emulsifier includes one or more of sodium lauryl sulfate, Tween 80, glyceryl monostearate, calcium dodecylbenzenesulfonate and polyoxyethylene styrene phenol formaldehyde resin.

[0014] In an optional embodiment, in the wettable powder, the weight ratio of fluopyram, fluazinam and triflumilast is 1:1 to 3:1.

[0015] In an optional embodiment, in the wettable powder, the weight ratio of fluopyram, fluazinam and triflumilast is 1:2:1.

[0016] In an optional embodiment, the particle size of the wettable powder of the fluorine-containing pesticide is 1 μm to 50 μm.

[0017] On the other hand, a method for preparing a wettable powder of a fluorine-containing pesticide is provided, the method comprising: mixing 20-90 parts of fluopyram, 10-80 parts of fluazinam, 10-80 parts of triflumilast, 10-60 parts of a surfactant, 0.1-5 parts of a stabilizer, 0.5-20 parts of an emulsifier, and the remainder of water, and stirring the mixture to obtain a wettable powder of the fluorine-containing pesticide.

[0018] In an optional embodiment, the wettable powder of the fluorine-containing pesticide is obtained by stirring evenly at a rotation speed of 300 r / h to 600 r / h.

[0019] The wettable powder of fluorine-containing pesticide and the preparation method thereof provided in the embodiment of the present invention have at least the following beneficial effects:

[0020] The wettable powder of fluorine-containing pesticide provided by the present invention is based on the compounding of fluopyram, fluazinam and triflurimidine amide, and the respective weight portions are limited. On the one hand, it can achieve the control of different harmful organisms, solve the problem of single action of pesticide components in the related art, and based on the setting of the weight portions of fluopyram, fluazinam and triflurimidine amide, it can not only target different harmful organisms, but also has good stability, and improves the medicinal properties of pesticides. The problems of large pesticide usage, high toxicity, serious environmental pollution, high residue and easy pathogenic bacteria to harm crops in existing pesticide products are solved. The wettable powder of fluorine-containing pesticide provided by the embodiment of the present invention has the advantages of improving the utilization rate of the agent (wettable powder of fluorine-containing pesticide of the present invention), significantly improving the biological control effect of pests and pathogens, reducing pesticide residues, reducing environmental pollution, and human and animal safety, and has potential market value. DETAILED DESCRIPTION

[0021] The embodiments of the present disclosure will be described in more detail below. However, it should be understood that the present disclosure can be implemented in various forms and should not be limited by the embodiments set forth herein. On the contrary, these embodiments are provided to make the present disclosure more thorough and complete, and to fully convey the scope of the present disclosure to those skilled in the art.

[0022] As used herein, the term "including" and its variations mean open inclusion, i.e., "including but not limited to". Unless otherwise stated, the term "or" means "and / or". The term "based on" means "based at least in part on". The terms "an example embodiment" and "an embodiment" mean "at least one example embodiment". The term "another embodiment" means "at least one additional embodiment". The terms "first", "second", etc. may refer to different or the same objects. Other explicit and implicit definitions may also be included below.

[0023] On the one hand, an embodiment of the present invention provides a wettable powder of a fluorine-containing pesticide, which comprises the following components in parts by weight: 20-90 parts of fluopyram, 10-80 parts of fluazinam, 10-80 parts of triflumilast, 10-60 parts of a surfactant, 0.1-5 parts of a stabilizer, 0.5-20 parts of an emulsifier, and the rest is water.

[0024] The wettable powder of fluorine-containing pesticide provided by the embodiment of the present invention can reduce the number of times pesticides are used, improve the utilization rate of pesticides, reduce environmental pollution and reduce toxicity to mammals, and solve the problems of existing pesticide products such as large pesticide usage, high toxicity, serious environmental pollution, high residue and easy pesticide damage to crops by pathogenic bacteria.

[0025] For example, the weight parts of fluopyram can be 20 parts, 30 parts, 40 parts, 50 parts, 60 parts, 70 parts, 80 parts or 90 parts, etc., the weight parts of fluazinam can be 10 parts, 20 parts, 30 parts, 40 parts, 50 parts, 60 parts, 70 parts or 80 parts, etc., the weight parts of triflurimidine can be 10 parts, 20 parts, 30 parts, 40 parts, 50 parts, 60 parts, 70 parts or 80 parts, etc., and the weight parts of surfactant can be 10 parts, 20 parts, 30 parts, 40 parts, 50 parts or 60 parts. The weight parts of the stabilizer can be 0.1 parts, 1.1 parts, 2 parts, 2.1 parts, 3 parts, 3.5 parts, 4.5 parts or 5 parts, etc., and the weight parts of the emulsifier can be 0.5 parts, 1.1 parts, 2 parts, 2.1 parts, 3 parts, 3.5 parts, 4 parts, 4.5 parts, 5 parts, 5.2 parts, 6 parts, 7 parts, 10 parts, 11.1 parts, 12 parts, 12.1 parts, 13 parts, 13.5 parts, 14 parts, 14.5 parts, 15 parts, 15.2 parts, 16 parts, 17 parts, 18 parts or 20 parts, etc.

[0026] In an optional embodiment, the wettable powder of the fluorine-containing pesticide comprises the following components in parts by weight: 20-70 parts of fluopyram, 10-50 parts of fluazinam, 10-50 parts of triflumilast, 10-40 parts of surfactant, 0.1-1 part of stabilizer, 0.5-10 parts of emulsifier, and the rest is water.

[0027] In an optional embodiment, the surfactant includes one or more of naphthalenesulfonate, woodsulfonate, alkylsulfonate, aminosulfonate, fatty alcohol salt, polyoxyethylene alkyl ether, modified naphthalenesulfonate, modified woodsulfonate, and modified aminosulfonate. The above-mentioned surfactant has high emulsifying power, wetting power, and penetrating power, and can make the wettable powder evenly suspended in water to form a uniform and stable suspension.

[0028] In an optional embodiment, the stabilizer includes one or more of pentaerythritol, an antioxidant and creatinine.

[0029] In an optional embodiment, the emulsifier includes one or more of sodium lauryl sulfate, Tween 80, glyceryl monostearate, calcium dodecylbenzenesulfonate and polyoxyethylene styrene phenol formaldehyde resin.

[0030] In an optional embodiment, in the wettable powder, the weight ratio of fluopyram, fluazinam and triflumilast is 1:1 to 3:1.

[0031] Exemplarily, the weight ratio of fluopyram, fluazinam, and triflumilast is 1:1.2:1, 1:2:1, 1:2.2:1, or 1:3:1, etc.

[0032] In an optional embodiment, in the wettable powder, the weight ratio of fluopyram, fluazinam and triflumilast is 1:2:1.

[0033] In an optional embodiment, the particle size of the wettable powder of the fluorine-containing pesticide is 1 μm to 50 μm.

[0034] Illustratively, the particle size of the wettable powder of the fluorine-containing pesticide can be 1 μm, 2 μm, 3 μm, 4 μm, 5 μm, 6 μm, 8 μm, 10 μm, 11 μm, 14 μm, 15 μm, 17 μm, 20 μm, 21 μm, 25 μm, 26 μm, 28 μm, 30 μm, 31 μm, 34 μm, 36 μm, 37 μm, 38 μm, 40 μm, 45 μm, 47 μm, 48 μm, 49 μm or 50 μm, etc.

[0035] On the other hand, a method for preparing a wettable powder of a fluorine-containing pesticide is provided, the method comprising: mixing 20-90 parts of fluopyram, 10-80 parts of fluazinam, 10-80 parts of triflumilast, 10-60 parts of a surfactant, 0.1-5 parts of a stabilizer, 0.5-20 parts of an emulsifier, and the remainder of water, and stirring the mixture to obtain a wettable powder of the fluorine-containing pesticide.

[0036] In an optional embodiment, the wettable powder of the fluorine-containing pesticide is obtained by stirring evenly at a rotation speed of 300 r / h to 600 r / h. For example, the wettable powder of the fluorine-containing pesticide can be obtained by stirring evenly at a rotation speed of 300 r / h, 350 r / h, 400 r / h, 450 r / h, 500 r / h, 550 r / h or 600 r / h.

[0037] The wettable powder of the fluorine-containing pesticide provided by the present invention will be further explained and illustrated by means of specific examples below.

[0038] Example 1

[0039] The wettable powder of the fluorine-containing pesticide provided in this embodiment includes 80 parts of fluopyram, 10 parts of fluazinam, 10 parts of triflumilast, 30 parts of a surfactant, 0.2 parts of a stabilizer and 0.8 parts of an emulsifier, and the rest is water.

[0040] Preparation method: Fluopyram, fluazinam and triflumizone are added into a three-in-one mixer according to the above ratio, and then a mixture of surfactants naphthalenesulfonate, wood sulfonate and alkyl sulfonate is added in a mixing ratio of 1:1:1. Stabilizer pentaerythritol and emulsifier sodium dodecyl sulfate are continuously mixed and stirred, and finally water is added and stirred evenly; the material is filtered to obtain the wettable powder of the fluorine-containing pesticide prepared in this embodiment.

[0041] Example 2

[0042] The wettable powder of the fluorine-containing pesticide provided in this embodiment includes 20 parts of fluopyram, 80 parts of fluazinam, 10 parts of triflumilast, 60 parts of surfactant, 1.5 parts of stabilizer, 0.5 parts of emulsifier and 0.05 parts of defoamer, and the rest is water.

[0043] Preparation method: Fluopyram, fluazinam and triflurimidine are added to a three-in-one mixer according to the above ratio, and then a mixture of a surfactant polyoxyethylene alkyl ether and a modified naphthalene sulfonate is added in a mixing ratio of 1:2, a mixture of a stabilizer antioxidant and creatinine is added in a mixing ratio of 1:2, and an emulsifier sodium lauryl sulfate is added and continued to mix and stir, and finally water is added and stirred evenly; the material is filtered to obtain the wettable powder of the fluorine-containing pesticide prepared in this embodiment.

[0044] Example 3

[0045] The wettable powder of the fluorine-containing pesticide provided in this embodiment includes 60 parts of fluopyram, 30 parts of fluazinam, 10 parts of triflumilast, 50 parts of surfactant, 1 part of stabilizer and emulsifier, and the rest is water.

[0046] Preparation method: Fluopyram, fluazinam and triflurimidine are added to a three-in-one mixer according to the above ratio, and then a mixture of a surfactant polyoxyethylene alkyl ether and a modified naphthalene sulfonate is added in a mixing ratio of 1:2, and a mixture of a stabilizer antioxidant and creatinine is added in a mixing ratio of 1:2, and an emulsifier sodium dodecyl sulfate is added, and the mixture is continued to be mixed and stirred, and the material is filtered to obtain the wettable powder of the fluorine-containing pesticide prepared in this embodiment.

[0047] Example 4

[0048] The wettable powder of the fluorine-containing pesticide provided in this embodiment includes 90 parts of fluopyram, 10 parts of fluazinam, 10 parts of triflumilast, 10 parts of surfactant, 0.1 parts of stabilizer, 20 parts of emulsifier, and the rest is water.

[0049] Preparation method: Fluopyram, fluazinam and triflurimidine are added into a three-in-one mixer according to the above ratio, and then a mixture of a surfactant polyoxyethylene alkyl ether and a modified naphthalene sulfonate is added in a mixing ratio of 1:2, and a mixture of a stabilizer antioxidant and creatinine is added in a mixing ratio of 1:2, and an emulsifier sodium dodecyl sulfate is added, and the mixture is continued to be mixed and stirred; the material is filtered to obtain the wettable powder of the fluorine-containing pesticide prepared in this embodiment.

[0050] Example 5

[0051] The wettable powder of the fluorine-containing pesticide provided in this embodiment includes 20 parts of fluopyram, 80 parts of fluazinam, 10 parts of other adjuvants, and the rest is water.

[0052] The surfactant is 0.5 parts of decaglycerol monooleate and 0.5 parts of bis-ethoxylated fatty alcohol polyoxyethylene ether; the antifreeze agent is propylene glycol, hexylene glycol, ethylene glycol, dimethylacetamide, and 3 parts of hexylene glycol; the stabilizer is urea, dimethylamine, dibenzoylmethane, benzotriazole, and 5 parts of toluenediamine;

[0053] The emulsifier is dibutyl secondary amine sulfate, alkylphenol polyoxyethylene ether and styrene phenyl polyoxyethylene ether, with 1 part of dibutyl secondary amine sulfate and a mixture of alkylphenol polyoxyethylene ether and styrene phenyl polyoxyethylene ether in a ratio of 1:3, and the total is 1 part.

[0054] Preparation method: Add fluopyram, fluazinam and triflumizone in a three-in-one mixer according to the above ratio, add part of the surfactant, stabilizer and emulsifier and continue to mix and stir, and finally add water and stir evenly; filter the material to obtain the wettable powder of the fluorine-containing pesticide prepared in this embodiment.

[0055] Application Examples

[0056] (1) Field test: Comparative test on the effect of eliminating the harm caused by highly toxic pesticides

[0057] Test drug: the drug of Examples 2, 3, 4, and 5 (wettable powder of the fluorine-containing pesticide of the present invention)

[0058] Test area: 40 acres

[0059] Test content: The test selected a small pond where aquatic organisms grew vigorously, and at 0 minutes, 50-60 kg of snails were scattered per mu. The test group was sprayed with a medicament (wettable powder of the fluorine-containing pesticide of the present invention) accounting for 80 parts of the snails' body weight at 0 minutes, and then the number of dead snails at 20 minutes, 40 minutes and 60 minutes was observed; the control group was only sprayed with an equal amount of clean water at 0 minutes; the test was repeated three times, and the mortality rate was calculated.

[0060] The mortality rates at 20 minutes, 40 minutes and 60 minutes were 14.3%, 31.6% and 42.1% respectively.

[0061] In this embodiment, when clean water was sprayed at 0 min, the mortality rates at 20 min, 40 min, and 60 min were 11.5, 25.3, and 33.7, respectively.

[0062] The comparison results show that when the spraying time is the same, the poisoning rate of snails in this embodiment is significantly improved. This is because the fluorine-containing pesticide in this embodiment is still active against snails at zero degrees Celsius, so that the snails can die quickly after being poisoned after spraying. At the same time, from the mortality rate, the snails are close to death after 20 minutes of spraying, which shows that the toxicity causes great harm to the target snails and has little effect on vegetables, thereby reducing the number of spraying and reducing the residue of the drug in the vegetables.

[0063] (2) Biodegradation test

[0064] Test method: Weigh 200 ml of the test concentration agent (wettable powder of the fluorine-containing pesticide of the present invention) and place it in 1000 ml of culture medium, and seal it in a conical flask; add 3-5 ml of inoculum, mix evenly, let it stand in a culture tank, take samples and culture regularly, and measure the concentration of active substances, and at the same time determine the degradation amount of active substances.

[0065] The test groups were: Examples 5, 6, 7, and 8 (wettable powders of the fluorine-containing pesticides of the present invention). The pH value of the test medium in the culture tank remained stable and did not change.

[0066] The control group was: Examples 5, 6, 7, and 8 (wettable powders of the fluorine-containing pesticides of the present invention). The culture medium in the culture tank was pH unstable and the culture medium was 5 parts of glucose solution.

[0067] Test results:

[0068] The drug prepared by the present invention has no change in the concentration of active matter within 3-5 days under static conditions at room temperature. Compared with the conventional 5-part glucose solution, the culture medium is a solution with unstable pH, and the active matter decreases rapidly and the downward trend is obvious, indicating that the components of the present application are relatively stable, less harmful to the environment, more conducive to protecting the ecological environment, and conducive to ecological circulation.

[0069] The embodiments of the present disclosure have been described above, and the above description is exemplary, not exhaustive, and is not limited to the disclosed embodiments. Many modifications and changes will be apparent to those of ordinary skill in the art without departing from the scope and spirit of the described embodiments. The selection of terms used herein is intended to best explain the principles of the embodiments, practical applications, or technical improvements in the market, or to enable other persons of ordinary skill in the art to understand the embodiments disclosed herein.

Claims

1. A wettable powder of a fluorine-containing pesticide, characterized in that: The wettable powder of the fluorine-containing pesticide comprises the following components in parts by weight: 20-90 parts of fluopyram, 10-80 parts of fluazinam, 10-80 parts of triflurimidine, 10-60 parts of surfactant, 0.1-5 parts of stabilizer, 0.5-20 parts of emulsifier, and the rest is water.

2. The wettable powder of fluorine-containing pesticide according to claim 1, characterized in that: The wettable powder of the fluorine-containing pesticide comprises the following components in parts by weight: 20-70 parts of fluopyram, 10-50 parts of fluazinam, 10-50 parts of triflumizone, 10-40 parts of surfactant, 0.1-1 part of stabilizer, 0.5-10 parts of emulsifier, and the rest is water.

3. The wettable powder of fluorine-containing pesticide according to claim 1 or 2, characterized in that: The surfactant includes one or more of naphthalenesulfonate, woodsulfonate, alkylsulfonate, aminosulfonate, fatty alcohol salt, polyoxyethylene alkyl ether, modified naphthalenesulfonate, modified woodsulfonate and modified aminosulfonate.

4. The wettable powder of fluorine-containing pesticide according to claim 1 or 2, characterized in that: The stabilizer includes one or more of pentaerythritol, antioxidant and creatinine.

5. The wettable powder of fluorine-containing pesticide according to claim 1 or 2, characterized in that: The emulsifier includes one or more of sodium lauryl sulfate, Tween 80, glyceryl monostearate, calcium dodecylbenzenesulfonate and styrylphenol formaldehyde resin polyoxyethylene ether.

6. The wettable powder of fluorine-containing pesticide according to claim 1 or 2, characterized in that: In the wettable powder, the weight ratio of fluopyram, fluazinam and triflumilast is 1:1 to 3:

1.

7. The wettable powder of the fluorine-containing pesticide according to claim 6, characterized in that: In the wettable powder, the weight ratio of fluopyram, fluazinam and triflumilast is 1:2:

1.

8. The wettable powder of fluorine-containing pesticide according to claim 1, characterized in that: The particle size of the wettable powder of the fluorine-containing pesticide is 1 μm to 50 μm.

9. A method for preparing a wettable powder of a fluorine-containing pesticide, characterized in that: The method comprises: mixing 20-90 parts of fluopyram, 10-80 parts of fluazinam, 10-80 parts of triflumizone, 10-60 parts of surfactant, 0.1-5 parts of stabilizer, 0.5-20 parts of emulsifier and the rest of water, and stirring evenly to obtain the wettable powder of the fluorine-containing pesticide.

10. The method for preparing a wettable powder of a fluorine-containing pesticide according to claim 9, characterized in that: The wettable powder of the fluorine-containing pesticide is obtained by stirring evenly at a rotation speed of 300 r / h to 600 r / h.