WO2021093269A1 - Nano aqueous agent comprising prochloraz and processing method therefor - Google Patents

Abstract

The present invention belongs to the technical field of pesticides, and discloses a nano aqueous agent comprising prochloraz. In the nano aqueous agent, the mass percentage content of prochloraz is 0.5%-10%, that of a surfactant is 5%-25%, and the balance is water. In the present invention, no organic solvent is included, and the nano aqueous agent is prepared by means of using surfactant micellar solubilization technology. Compared with conventional pesticide formulations, the nano aqueous agent has excellent stability, and is still stable after cold storage at 0°C for 7 days and hot storage at 54°C for 14 days, chlorpyrifos is not precipitated, which facilitates storage, and same has a longer shelf life. The nano aqueous agent of the present invention has lower production costs, better fast-acting performance and long-acting performance, has no adverse reactions such as drug damage, and is more suitable for application by an unmanned aerial vehicle.

Description

Nano water agent containing prochloraz and its processing method Technical field

The invention belongs to the technical field of pesticide production and processing, and specifically relates to a new formulation containing prochloraz-a nano-aqueous agent and a processing method thereof.

Background technique

Prochloraz is a broad-spectrum fungicide, molecular formula: C ₁₅ H ₁₆ Cl ₃ N ₃ O ₂ , chemical name: N-propyl-N-[2-(2,4,6-trichlorobenzene (Oxy)ethyl]-imidazole-1-carboxamide. Prochloraz has obvious control effects on various crops caused by ascomycetes and deuteromycetes. It can also be mixed with most fungicides, insecticides, and herbicides, and has good control effects. It has the effect of curing and eradicating various diseases on field crops, fruits and vegetables, turf and ornamental plants.

Prochloraz is difficult to dissolve in water, and its solubility in water at 25°C is only 5.5mg/L. At present, the pesticide formulations developed with prochloraz as the original drug are mainly emulsifiable concentrates and water emulsions, etc. Both emulsifiable concentrates and water emulsions contain a large amount of organic solvents. In the process of use, organic solvents not only cause serious harm to the environment, but also seriously affect the quality of agricultural products, accelerate food safety crisis, and endanger human health.

With the continuous improvement of users' awareness of environmental protection and the rapid growth of demand for sanitary drugs, the existing dosage forms of prochloraz cannot meet the needs of use. In order to ensure that under the premise of safety and environmental protection, accelerate the promotion and use of prochloraz products, it is particularly necessary to develop a new formulation that is friendly to humans, animals and the environment, and facilitates the application of aerial plant protection technologies and equipment such as drones.

Summary of the invention

In response to the above-mentioned technical problems, the inventors screened out specific surfactants. Under the condition of no organic solvents, the surfactants are used to form nano-sized micelles with an average particle size for carrying pesticides that are difficult to dissolve in water. Xanthan amine can be used as a water agent to form a new type of pesticide nano water agent.

The purpose of the present invention is achieved through the following technical solutions:

A nano-aqueous agent containing prochloraz, which only uses prochloraz technical, surfactant and water as raw materials, and is made by using surfactant micellar solubilization technology. The nano-aqueous agent does not contain any organic solvents; , The mass percentage of the active ingredient prochloraz is 0.5-25%, the mass percentage of the surfactant is 3-25%, and the balance is water.

Preferably, in the nano-aqueous agent, the mass percentage of the prochloraz is 1-10%, the mass percentage of the surfactant is 3-25%, and the balance is water.

Said surfactant is selected from fatty alcohol polyoxyethylene ether, alkylphenol formaldehyde resin polyoxyethylene ether, styrylphenol polyoxyethylene ether, fatty alcohol polyoxyethylene ether phosphate, tristyrylphenol polyoxyethylene One or more combinations of vinyl ether phosphate, sodium fatty acid methyl sulfonate, sodium alcohol ether succinate monoester sulfonate, and sorbitan fatty acid ester polyoxyethylene ether.

Another object of the present invention is to provide a method for preparing a prochloraz-containing nano-aqueous agent. The prochloraz original drug is mixed with a surfactant, and then water is added and stirred to form a surfactant micellar solution, which is Nano water agent containing prochloraz.

Specifically, the preparation method of the prochloraz-containing nano-aqueous agent includes the following steps:

Step (1), at room temperature (10-35°C), mix the prochloraz technical agent and the surfactant, and stir, so that the prochloraz is uniformly dispersed in the surfactant;

Step (2), adding water and stirring uniformly to form a surfactant micelle solution, which is the prochloraz nano-aqueous agent.

Preferably, in step (1), the stirring speed is 60-100 revolutions per second, and the stirring time is based on the uniform dispersion of prochloraz in the surfactant, generally 0.5 h.

Preferably, in step (2), the stirring speed is 60-100 revolutions per second, and the stirring time is 0.5-1 h.

Compared with the conventional conventional pesticide water formulations, the effective ingredients in the nano water formulations of the present invention are insoluble in water and cannot form a true true solution. Instead, they are coated by nano-scale surfactant micelles and uniformly dispersed in the water to form a true true solution. Solution. The prochloraz-containing nano-aqueous agent of the present invention is a light yellow transparent liquid, which can be quickly dissolved in water after entering water to form a completely transparent solution, and the dilution stability is qualified, and it is more suitable for drone application technology.

The prochloraz-containing nano-aqueous agent of the present invention can be widely used in the prevention and treatment of various fungal diseases on field crops, fruits and vegetables, turf and ornamental plants, such as rice blast, wheat sheath blight, and pepper anthracnose, and Compared with the existing emulsifiable concentrates, the nano-aqueous agent of the present invention has excellent quick-acting properties, and the prochloraz in the nano-aqueous agent exists as nano-sized particles, which is more convenient for its attachment, spreading and penetration on the target, and is more resistant to rain erosion. It has excellent lasting effect, and under the premise of the same application amount, the control effect of the nano-aqueous agent of the present invention is significantly higher than that of the same period of 25% prochloraz emulsifiable concentrate, and the drug effect is better.

The particle size detection method of the nano-aqueous agent of the present invention: the particle size of the surfactant micelles in the pesticide nano-aqueous agent is measured (25°C) by using the Malvern high-sensitivity nano particle size analyzer Zetasizer NanoS.

Compared with the prior art, the present invention has the following beneficial effects:

1. The prochloraz nano-aqueous agent of the present invention does not contain any organic solvents, is safe and environmentally friendly, and belongs to an environment-friendly dosage form. It is not only suitable for agricultural medicine, but also suitable for sanitary medicine needs, and can be widely used in agriculture, households and public health.

2. The present invention has low production cost, simple processing technology and very good economy.

3. The active ingredients of the present invention are carried by nano-scale micelles, which can form a true solution, and the preparation is more stable. It is still stable after cold storage at 0°C for 7 days and 54°C hot storage for 14 days. Prochloraz does not precipitate and is convenient for storage. Longer period.

4. The present invention is a nano-preparation product with extremely small drug fineness, no particle precipitation, and better drug effect.

Description of the drawings

Fig. 1 shows the state of the 6% prochloraz nano-aqueous preparation prepared in Example 6 after being placed at a low temperature (0° C.) for 1-2 days and then heated to room temperature.

Figure 2 shows the state of the 6% prochloraz solution prepared at room temperature in Comparative Example 4 after being placed at low temperature (0°C) for 1-2 days and then heated to room temperature.

Detailed ways

The present invention will be further described below in conjunction with examples, but the protection scope of the present invention is not limited to this:

Example 1

Preparation method: Weigh 10g prochloraz prochloraz (based on the ingredients, the same below), 80g styrylphenol polyoxyethylene ether and 20g alkylphenol formaldehyde resin polyoxyethylene ether according to the dosage, and mix the three Afterwards, stirring was carried out at 100 revolutions per second for 0.5 h, 890 g of water was added under stirring, and stirring was continued for 1 h to obtain 1% prochloraz nano-aqueous agent.

The nano-aqueous agent of this example has a slightly yellow and transparent appearance, a viscosity of 105 mPa·s, and an average particle size of 12.0 nanometers. After entering water, the nano-aqueous agent of this embodiment can quickly dissolve with water to form a completely transparent solution, and the dilution stability is qualified.

After the nano-aqueous agent of this example was stored at 0°C for 7 days and 54°C for 14 days, there was no precipitation phenomenon, and it was still stable.

Example 2

The preparation method is the same as in Example 1, and the 2% prochloraz nano-aqueous agent is prepared.

The nano-aqueous agent of this example is transparent and colorless in appearance, has a viscosity of 86 mPa·s, and an average particle size of 14.7 nanometers. After entering water, the nano-aqueous agent of this embodiment can quickly dissolve with water to form a completely transparent solution, and the dilution stability is qualified.

After the nano-aqueous agent of this example was stored at 0°C for 7 days and 54°C for 14 days, there was no precipitation phenomenon, and it was still stable.

Example 3

The preparation method is the same as in Example 1, and 3% prochloraz nano-aqueous agent is prepared.

The nano-aqueous agent of this example has a slightly yellow and transparent appearance, a viscosity of 95 mPa·s, and an average particle size of 17.8 nanometers. After entering water, the nano-aqueous agent of this embodiment can quickly dissolve with water to form a completely transparent solution, and the dilution stability is qualified.

After the nano-aqueous agent of this example was stored at 0°C for 7 days and 54°C for 14 days, there was no precipitation phenomenon, and it was still stable.

Example 4

The preparation method is the same as in Example 1, and 4% prochloraz nano-aqueous agent is prepared.

The nano-aqueous agent of this embodiment has a slightly yellow and transparent appearance, a viscosity of 78 mPa·s, and an average particle size of 19.5 nanometers. After entering water, the nano-aqueous agent of this embodiment can quickly dissolve with water to form a completely transparent solution, and the dilution stability is qualified.

After the nano-aqueous agent of this example was stored at 0°C for 7 days and 54°C for 14 days, there was no precipitation phenomenon, and it was still stable.

Example 5

The preparation method is the same as in Example 1, and the 5% prochloraz nano-aqueous agent is prepared.

The nano-aqueous agent of this example has a slightly yellow and transparent appearance, a viscosity of 80 mPa·s, and an average particle size of 21.7 nanometers. After entering water, the nano-aqueous agent of this embodiment can quickly dissolve with water to form a completely transparent solution, and the dilution stability is qualified.

After the nano-aqueous agent of this example was stored at 0°C for 7 days and 54°C for 14 days, there was no precipitation phenomenon, and it was still stable.

Example 6

The preparation method is the same as in Example 1, and the 6% prochloraz nano-aqueous agent is prepared.

The nano-aqueous agent of this example has a slightly yellow and transparent appearance, a viscosity of 76 mPa·s, and an average particle size of 23.6 nanometers. After entering water, the nano-aqueous agent of this embodiment can quickly dissolve with water to form a completely transparent solution, and the dilution stability is qualified.

After the nano-aqueous agent of this example was stored at 0°C for 7 days and 54°C for 14 days, there was no precipitation phenomenon, and it was still stable. As shown in Figure 1, the 6% prochloraz nano-aqueous agent is placed at 0°C for 1-2 days and then heated to room temperature. The appearance is still slightly yellow and transparent without precipitation.

Example 7

The preparation method is the same as in Example 1, and the 7% prochloraz nano-aqueous agent is prepared.

The nano-aqueous agent of this example has a slightly yellow and transparent appearance, a viscosity of 78 mPa·s, and an average particle size of 24.1 nanometers. After entering water, the nano-aqueous agent of this embodiment can quickly dissolve with water to form a completely transparent solution, and the dilution stability is qualified.

After the nano-aqueous agent of this example was stored at 0°C for 7 days and 54°C for 14 days, there was no precipitation phenomenon, and it was still stable.

Example 8

The preparation method is the same as in Example 1, and a 9% prochloraz nano-aqueous agent is prepared.

The nano-aqueous agent of this example has a slightly yellow and transparent appearance, a viscosity of 67 mPa·s, and an average particle size of 23.7 nanometers. After entering water, the nano-aqueous agent of this embodiment can quickly dissolve with water to form a completely transparent solution, and the dilution stability is qualified.

After the nano-aqueous agent of this example was stored at 0°C for 7 days and 54°C for 14 days, there was no precipitation phenomenon, and it was still stable.

Example 9

The preparation method is the same as in Example 1, and the 10% prochloraz nano-aqueous agent is prepared.

The nano-aqueous agent of this example has a slightly yellow and transparent appearance, a viscosity of 80 mPa·s, and an average particle size of 20.4 nanometers. After entering water, the nano-aqueous agent of this embodiment can quickly dissolve with water to form a completely transparent solution, and the dilution stability is qualified.

After the nano-aqueous agent of this example was stored at 0°C for 7 days and 54°C for 14 days, there was no precipitation phenomenon, and it was still stable.

Comparative example 1-Comparative example 4

Conventional additives (wetting agents) were used for the preparation experiment of the water agent, and the specific formula is shown in Table 1.

Table 1. Formulations of Comparative Example 1-Comparative Example 4

The raw materials were weighed according to the formulas of Comparative Example 1 and Comparative Example 2, and the preparation method of Example 1 was adopted. With the addition of additives, the prochloraz still could not be completely dissolved in water and could not form a qualified aqueous solution. According to the formulations of Comparative Example 3 and Comparative Example 4, the raw materials were weighed, and the preparation method of Example 1 was used to prepare an aqueous solution at room temperature (10-35°C), but the aqueous solution was placed at low temperature (below 0°C). Prochloraz will continue to precipitate out and cannot be recovered after heating up (see Figure 2). It shows that the use of surfactants used in conventional water agents other than the surfactants of the present invention cannot be used to prepare qualified prochloraz nano-aqueous agents.

Example 11 Biological Activity Comparison

Field efficacy test one:

Test agent: the prochloraz nano-aqueous prepared in Example 1 to Example 9.

Control agent: 25% prochloraz EC (commercially available).

Control object: rice blast.

experiment method:

1. Test treatment: The dosage of this test agent is set at three treatment concentrations according to the difference of each component. The control agent is a pesticide single agent 25% prochloraz EC and a blank water test.

2. Test method: The area of each plot is 66.7m ² , repeated 3 times; the survey before spraying and the survey efficacy method after control are: randomly sample 5 points in the experimental treatment area (each point is 5m ² ), According to the relevant standards of national field trials, the disease is classified and the control effect is calculated.

3. See the following table for the test results:

Table 2. Field test effects of the preparations of the present invention on the control of rice blast

It can be seen from the above table that the prochloraz nano-aqueous agent has shown excellent quick-acting and sustained-effect in the prevention and control of rice blast, and the lasting effect is more than one month. During the experiment, no adverse reactions such as drug damage were found, which has practical application value.

Field efficacy test two:

Test agent: the prochloraz nano-aqueous prepared in Example 1 to Example 9.

Control agent: 25% prochloraz EC (commercially available).

Control object: Pepper anthracnose.

experiment method:

1. Test treatment: The dosage of this test agent is set at three treatment concentrations according to the difference of each component. The control agent is a pesticide single agent 25% prochloraz EC and a blank water test.

2. Test method: The area of each plot is 66.7m ² , repeated 3 times; the survey before spraying and the survey efficacy method after control are: randomly sample 5 points in the experimental treatment area (each point is 5m ² ), According to the relevant standards of national field trials, the disease is classified and the control effect is calculated.

3. See the following table for the test results:

Table 3. Field test effects of the preparations of the present invention on controlling pepper anthracnose

From the above table, it can be seen that the prochloraz nano-aqueous agent has shown excellent quick-acting and lasting effect in the prevention and control of pepper anthracnose, and the lasting period is more than one month. During the experiment, no adverse reactions such as drug damage were found, which has practical application value.

Claims (6)

1. A nano-aqueous agent containing prochloraz, which is characterized in that the nano-aqueous agent is made of prochloraz original medicine, surfactant and water as raw materials, and is made by using surfactant micellar solubilization technology; among them, prochloraz The mass percentage of amine is 0.5-25%, the mass percentage of surfactant is 3-25%, and the balance is water.
2. The nano-aqueous agent containing prochloraz according to claim 1, characterized in that the mass percentage of the prochloraz is 1-10%, and the mass percentage of the surfactant is 3-25%, The balance is water.
3. The prochloraz-containing nano-aqueous agent according to claim 1, wherein the surfactant is selected from fatty alcohol polyoxyethylene ether, alkylphenol formaldehyde resin polyoxyethylene ether, styrylphenol polyoxyethylene Vinyl ether, fatty alcohol polyoxyethylene ether phosphate, tristyryl phenol polyoxyethylene ether phosphate, sodium fatty acid methyl sulfonate, sodium alcohol ether succinate monoester sulfonate, sorbitan fatty acid ester polyoxyethylene One or more combinations of vinyl ether.
4. The processing method of the prochloraz-containing nano-aqueous agent according to claim 1, characterized in that the prochloraz original drug is mixed with a surfactant, and then water is added and stirred to form a surfactant micellar solution, which is a solution containing prochloraz. The nano-aqueous agent of prochloraz.
5. The processing method of prochloraz-containing nano-aqueous agent according to claim 4, characterized in that it comprises the following steps:

   Step (1), at room temperature, mix the prochloraz technical agent and the surfactant, and stir, so that the prochloraz is uniformly dispersed in the surfactant;

   Step (2), adding water and stirring uniformly to form a surfactant micelle solution, which is the prochloraz nano-aqueous agent.
6. The method for processing prochloraz-containing nano-aqueous agent according to claim 4, characterized in that in step (1), the stirring speed is 60-100 revolutions per second; in step (2), the stirring speed is 60-100 Revolutions per second.

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