阅读说明：本技术 多效唑水乳剂及其制备方法和应用 (Paclobutrazol aqueous emulsion and preparation method and application thereof ) 是由 张贵森 张宝俊 段杨波 郭慧玲 路容菲 于 2019-10-10 设计创作，主要内容包括：本申请涉及植物生长调节剂技术领域,公开一种多效唑水乳剂方法,以质量百分含量计,所述水乳剂包括：多效唑8-12％；有机溶剂30-45％；乳化剂8-13％；水补足100％。本公开实施例提供的多效唑水乳剂提高了多效唑对植物生长的调节作用。本申请还公开了一种多效唑水乳剂的制备方法和应用。(The application relates to the technical field of plant growth regulators, and discloses a method for preparing paclobutrazol emulsion in water, which comprises the following steps of: 8-12% of paclobutrazol; 30-45% of organic solvent; 8-13% of emulsifier; water makes up to 100%. The paclobutrazol aqueous emulsion provided by the embodiment of the disclosure improves the regulating effect of paclobutrazol on plant growth. The application also discloses a preparation method and application of the paclobutrazol aqueous emulsion.)

1. The paclobutrazol aqueous emulsion is characterized by comprising the following components in percentage by mass:

2. the aqueous emulsion of claim 1,

the organic solvent comprises N, N-dimethyldecanamide.

3. The aqueous emulsion of claim 1, wherein the emulsifier comprises one or a combination of more than one of the following:

sorbitan laurate, phosphate ester compounds and acrylic copolymer potassium salt.

4. The aqueous emulsion of claim 3, characterized in that the emulsifier comprises sorbitan laurate and phosphate compounds,

wherein the mass ratio of the sorbitan laurate to the phosphate ester compound is 8-10: 1.

5. The aqueous emulsion of claim 4,

the mass ratio of the sorbitan laurate to the phosphate ester compound is 9: 1.

6. The aqueous emulsion of claim 1,

in the aqueous emulsion, the mass percentage of the emulsifier is 10%.

7. A preparation method of paclobutrazol aqueous emulsion is characterized by comprising the following steps:

mixing paclobutrazol and an organic solvent, and dissolving to obtain an oil phase;

mixing an emulsifier with water to obtain a water phase;

mixing the oil phase and the water phase, and then carrying out emulsification treatment to obtain the paclobutrazol aqueous emulsion of any one of claims 1 to 6.

8. The method for preparing according to claim 7, wherein the emulsification treatment comprises:

the emulsification treatment is carried out at a rotation speed of 10000r/min, and the shearing time is 100-150 seconds.

9. Use of a paclobutrazol aqueous emulsion according to any one of claims 1 to 6 for regulating plant growth.

10. Use according to claim 9, wherein the plant comprises cucumber, peanut, wheat, rice.

Technical Field

The application relates to the technical field of plant growth regulators, for example to a paclobutrazol water emulsion and a preparation method and application thereof.

Background

The Plant Growth Regulator can be used for regulating the Growth and storage of fruits and vegetables, and plays an important role in improving the yield and quality of agricultural products in the agricultural production process.

Paclobutrazol (Paclobutrazol) is a plant growth regulator developed by British chemical company in the end of the 70 th 20 th century, is a high-efficiency and low-toxicity growth retardant, and can reduce the content of gibberellin and indoleacetic acid in crops, increase the release amount of ethylene, improve the stress resistance of crops such as lodging resistance, drought resistance and the like, increase the yield and improve the quality of the crops.

In the process of implementing the embodiments of the present disclosure, it is found that at least the following problems exist in the related art: there is no description of paclobutrazol aqueous emulsions.

Disclosure of Invention

The following presents a simplified summary in order to provide a basic understanding of some aspects of the disclosed embodiments. This summary is not an extensive overview nor is intended to identify key/critical elements or to delineate the scope of such embodiments but rather as a prelude to the more detailed description that is presented later.

The embodiment of the disclosure provides a paclobutrazol emulsion in water, a preparation method and an application thereof, which aim to solve the technical problem that no record is provided for the paclobutrazol emulsion in water.

In some embodiments, the paclobutrazol aqueous emulsion includes, by mass percent: 8-12% of paclobutrazol; 30-45% of organic solvent; 8-13% of emulsifier; water makes up to 100%.

In some embodiments, the preparation method of the paclobutrazol aqueous emulsion comprises the following steps: mixing paclobutrazol and an organic solvent, and dissolving to obtain an oil phase; mixing an emulsifier with water to obtain a water phase; and mixing the oil phase and the water phase, and emulsifying to obtain the paclobutrazol water emulsion.

In some embodiments, the aforementioned paclobutrazol aqueous emulsions are used to regulate plant growth.

The paclobutrazol emulsion in water, the preparation method and the application thereof provided by the embodiment of the disclosure can realize the following technical effects:

in the paclobutrazol aqueous emulsion provided by the embodiment of the disclosure, the paclobutrazol crude drug is 8-12% by mass, the organic solvent is 30-45% by mass, the emulsifier is 8-13% by mass, and finally water is added to make up 100% to obtain the paclobutrazol aqueous emulsion with good stability and good regulation effect on plant growth.

The foregoing general description and the following description are exemplary and explanatory only and are not restrictive of the application.

Detailed Description

So that the manner in which the features and technical content of the embodiments of the present disclosure can be understood in detail, a detailed description of the embodiments of the present disclosure will be provided below. In the following description of the technology, for purposes of explanation, numerous details are set forth in order to provide a thorough understanding of the disclosed embodiments. However, one or more embodiments may be practiced without these details.

The embodiment of the disclosure provides a paclobutrazol aqueous emulsion, which comprises the following components in percentage by mass: 8-12% of paclobutrazol; 30-45% of organic solvent; 8-13% of emulsifier; water makes up to 100%.

The emulsion in water provided by the embodiment of the disclosure takes paclobutrazol as a raw pesticide. Alternatively, the paclobutrazol may be 95% paclobutrazol, by mass percentage. The weight percentage of the paclobutrazol in the aqueous emulsion is 8-12 percent, which can be understood as that the paclobutrazol crude drug in the aqueous emulsion is 8-12 percent. Optionally, the percentage by mass of paclobutrazol in the aqueous emulsion may be 8%, 9%, 10%, 11%, 12%, and a range value composed of these values.

Optionally, the mass percentage of the organic solvent in the paclobutrazol water emulsion can be 30%, 33%, 35%, 37%, 39%, 40%, 41%, 43%, 45% and the range value formed by the numerical values; the percentage by mass of emulsifier can be 8%, 9%, 10%, 11%, 12%, 13%, and ranges of values made up of these values.

According to the embodiment of the disclosure, the weight percentage of the original medicine, the organic solvent and the emulsifier in the paclobutrazol aqueous emulsion is limited, so that the obtained paclobutrazol aqueous emulsion with good parameters of hot storage, cold storage and the like has a good regulation effect on plant growth.

Alternatively, the organic solvent comprises N, N-dimethyldecanamide.

The organic solvent in the paclobutrazol water emulsion can be N, N-dimethyl capramide, so that the dissolving effect of paclobutrazol raw medicines is improved. Optionally, the organic solvent comprises N, N-dimethyldecanamide and a cosolvent, wherein the cosolvent may be one or a combination of more than one of cyclohexanone, toluene and xylene, so as to improve the dissolving effect on the paclobutrazol crude drug. Alternatively, when the organic solvent comprises N, N-dimethyldecanamide and a co-solvent, the mass ratio of N, N-dimethyldecanamide to co-solvent is 9-10: 1. Namely, the mass ratio of N, N-dimethyldecanamide in an organic solvent: cosolvent is 9-10: 1.

Optionally, the emulsifier comprises one or more of sorbitan laurate, phosphate compound and acrylic copolymer potassium salt.

Sorbitan laurate, also known as span-20, is a nonionic surfactant; the phosphate ester compound may be a phosphate polymer, wherein the phosphate polymer may also be referred to as a polyphosphate, for example, the phosphate esters CF-20S produced by Haian petrochemical plants of Jiangsu province, phosphate ester polymers [ J ] described in polyurethane industry, 1980(03): 46.

Optionally, in the emulsifier, the mass ratio of the sorbitan laurate to the phosphate ester compound is 8-10:1, that is, the ratio of the sorbitan laurate to the phosphate ester compound is, by mass: the phosphate ester compound is 8-10: 1.

In the paclobutrazol water emulsion, the emulsifier comprises sorbitan laurate and phosphate compounds, so that the emulsifying effect of paclobutrazol is improved, wherein the mass ratio of the sorbitan laurate to the phosphate compounds in the emulsifier can be 8:1, 9:1 or 10: 1.

Optionally, when the mass ratio of the sorbitan laurate to the phosphate ester compound in the emulsifier is 8-10:1, the heat storage stability of the paclobutrazol water emulsion is improved.

The heat storage stability of the paclobutrazol water emulsion is measured by referring to the national standard GB/T19136-2003 'measuring method for the heat storage stability of pesticide'. 10mL of a sample to be tested is put into a centrifuge tube, and the centrifuge tube is placed in a GZX-DF-II type electrothermal blowing dry box (Shanghai-Hengchang scientific instruments Co., Ltd.) at the temperature of (54 +/-2) DEG C for storage for 14 days, and then the appearance change of the sample to be tested is observed. If the oil is not separated out and the water separation rate is lower than 10 percent, the product is qualified. According to observation, the paclobutrazol water emulsion with the mass ratio of the sorbitan laurate to the phosphate ester compound in the emulsifier of 8-10:1 has no oil precipitation phenomenon, the water precipitation rate is less than 10 percent, and the heat storage is qualified.

Optionally, when the mass ratio of the sorbitan laurate to the phosphate ester compound in the emulsifier is 8-10:1, the cold storage stability of the paclobutrazol emulsion in water is improved.

The cold storage stability of the paclobutrazol water emulsion is measured by referring to the national standard GB/T19137-2003 'method for measuring the low-temperature stability of pesticide'. And (3) putting 10mL of sample to be detected into a centrifuge tube, storing the sample in a refrigerator at 0 ℃ for 14 days, and observing the appearance change of the sample to be detected. If no water, no oil, no layering and no precipitation are generated, the product is qualified. According to observation, the paclobutrazol water emulsion with the mass ratio of the sorbitan laurate to the phosphate ester compound in the emulsifier of 8-10:1 has no phenomena of water separation, oil separation, layering and precipitation, and is qualified in cold storage.

Optionally, when the mass ratio of the sorbitan laurate to the phosphate ester compound in the emulsifier is 8-10:1, the particle size of the paclobutrazol emulsion in water is reduced, and the uniformity of the particle size of the paclobutrazol emulsion in water is improved.

The method comprises the steps of performing particle size determination on five samples, namely a paclobutrazol emulsion in water 1, a paclobutrazol emulsion in water 2, a paclobutrazol emulsion in water 3, a paclobutrazol emulsion in water 4 and a paclobutrazol emulsion in water 5, by using a WJL-602 type laser particle size analyzer (Shanghai apparatus electro-physical optical instruments Co., Ltd.), performing parallel determination for 3 times and recording, wherein an absolute difference value is less than 0.1, and finally taking an arithmetic mean value of the samples as a particle size value of the samples.

The paclobutrazol water emulsion 1 comprises the following components in percentage by mass: 10% of paclobutrazol; 40% of N, N-dimethyldecanamide; 3% of sorbitan laurate; 7% of phosphate compound; water makes up to 100%.

The paclobutrazol water emulsion 2 comprises the following components in percentage by mass: 10% of paclobutrazol; 40% of N, N-dimethyldecanamide; 5% of sorbitan laurate; 5% of phosphate compounds; water makes up to 100%.

The paclobutrazol water emulsion 3 comprises the following components in percentage by mass: 10% of paclobutrazol; 40% of N, N-dimethyldecanamide; 6% of sorbitan laurate; 4% of phosphate compound; water makes up to 100%.

The paclobutrazol water emulsion 4 comprises the following components in percentage by mass: 10% of paclobutrazol; 40% of N, N-dimethyldecanamide; 8% of sorbitan laurate; 2% of phosphate compounds; water makes up to 100%.

The paclobutrazol water emulsion 5 comprises the following components in percentage by mass: 10% of paclobutrazol; 40% of N, N-dimethyldecanamide; 9% of sorbitan laurate; 1% of phosphate compound; water makes up to 100%.

Through measurement, D of paclobutrazol water emulsion 1₅₀13.47 μm, D₉₀28.63 μm, D₁₀5.02 μm; paclobutrazol water emulsion 2D₅₀Is 14.04 μm, D₉₀27.37 μm, D₁₀6.19 μm; paclobutrazol water emulsion 3D₅₀9.29 μm, D₉₀19.25 μm, D₁₀Is 4.04 μm; paclobutrazol water emulsion 4D₅₀Is 7.66 μm, D₉₀17.51 μm, D₁₀2.90 μm; paclobutrazol water emulsion 5D₅₀Is 3.37 μm, D₉₀Is 10.12 μm, D₁₀It was 1.34 μm. It can be seen that the paclobutrazol water emulsion 5 has a narrow particle size range and a minimum average particle size. When the mass ratio of the sorbitan laurate: phosphate ester compound ═ 8:1, or, sorbitan laurate: when the phosphate compound is 10:1, the particle size value of the obtained paclobutrazol aqueous emulsion is the same as or similar to that of the paclobutrazol aqueous emulsion 5.

Optionally, when the mass ratio of the sorbitan laurate to the phosphate ester compound in the emulsifier is 8-10:1, the wettability and the fluidity of the paclobutrazol aqueous emulsion are improved.

Using an instrument LVDV-2 digital viscometer (Shanghai Cyanini instruments, Inc.) for measuring viscosity, performing viscosity measurement on five samples, namely the paclobutrazol water emulsion 1, the paclobutrazol water emulsion 2, the paclobutrazol water emulsion 3, the paclobutrazol water emulsion 4 and the paclobutrazol water emulsion 5, wherein the value taking method is the same as the particle size measurement, and performing parallel measurement for 3 times to take the arithmetic average value as the effective viscosity value of the sample.

Through measurement, the viscosity of the paclobutrazol aqueous emulsion 1 is 152.33 Pascal seconds, the viscosity of the paclobutrazol aqueous emulsion 2 is 202.90 Pascal seconds, the viscosity of the paclobutrazol aqueous emulsion 3 is 181.33 Pascal seconds, the viscosity of the paclobutrazol aqueous emulsion 4 is 133.87 Pascal seconds, and the viscosity of the paclobutrazol aqueous emulsion 5 is 132.60 Pascal seconds. It can be seen that when the emulsifier is sorbitan laurate and phosphate ester compounds, the viscosity of the paclobutrazol aqueous emulsion is in the range of 132-203 pascal-seconds, wherein the paclobutrazol aqueous emulsion 5 has good wettability and fluidity. When the mass ratio of the sorbitan laurate: phosphate ester compound ═ 8:1, or, sorbitan laurate: when the phosphate compound is 10:1, the viscosity value of the obtained paclobutrazol aqueous emulsion is the same as or similar to that of the paclobutrazol aqueous emulsion 5.

Optionally, when the emulsifier is a mixture of sorbitan laurate and phosphate ester compounds, the stability of the pH value of the paclobutrazol aqueous emulsion is improved.

And (3) measuring the pH values of the paclobutrazol aqueous emulsion 1, the paclobutrazol aqueous emulsion 2, the paclobutrazol aqueous emulsion 3, the paclobutrazol aqueous emulsion 4 and the paclobutrazol aqueous emulsion 5 by using a pH meter, at least parallelly measuring for 3 times, wherein the absolute difference value of each measured result is less than 0.1, and taking the arithmetic mean value of the absolute difference values as the pH value of the sample.

Through measurement, the pH value of the paclobutrazol emulsion in water 1 is 7.70, the pH value of the paclobutrazol emulsion in water 2 is 7.69, the pH value of the paclobutrazol emulsion in water 3 is 7.70, the pH value of the paclobutrazol emulsion in water 4 is 7.69, and the pH value of the paclobutrazol emulsion in water 5 is 7.76. Therefore, when the emulsifier is a mixture of sorbitan laurate and phosphate ester compounds, the pH value of the obtained paclobutrazol aqueous emulsion tends to be stable.

Optionally, when the mass percentage of the sorbitan laurate to the phosphate ester compound in the emulsifier is 8-10:1, the stability of the paclobutrazol water emulsion is improved.

The stability of the paclobutrazol aqueous emulsion 5 is measured by referring to the national standard GB/T1603-2001 'method for measuring the stability of pesticide emulsion'. 10ml of the sample is taken and diluted to 200ml by adding water, and the sample is placed in a glass test tube with a plug and kept stand for 1h in an electric heating constant-temperature water bath kettle at the temperature of 30 ℃ to observe the appearance. If the emulsion appearance is kept uniform under the specified test conditions, no sediment or floating oil is separated out, the emulsion is qualified; if the emulsion is not uniform in appearance, or precipitates or oil slicks are precipitated, the emulsion is not qualified. Through measurement, the paclobutrazol water emulsion 5 has the advantages of uniform appearance, no precipitation, no floating oil precipitation and good stability.

Optionally, in the aqueous emulsion, the weight percentage of the emulsifier is 10%, so that the regulation effect of the paclobutrazol aqueous emulsion on the growth of plants is improved.

The embodiment of the disclosure also provides a preparation method of the paclobutrazol aqueous emulsion, which comprises the following steps:

mixing paclobutrazol and an organic solvent, and dissolving to obtain an oil phase; mixing an emulsifier with water to obtain a water phase; and mixing the oil phase and the water phase, and emulsifying to obtain the paclobutrazol water emulsion. Optionally, the emulsification treatment comprises: the emulsification treatment is carried out at the rotating speed of 10000r/min, the shearing time is 100-150 seconds, and the stability of the prepared paclobutrazol water emulsion is improved.

The embodiment of the disclosure also provides an application of the paclobutrazol water emulsion, which is used for regulating the growth of plants. Optionally, the paclobutrazol water emulsion provided by the embodiment of the disclosure is used for regulating the growth of cucumbers.

The indoor activities of the paclobutrazol water emulsion 5 and the control agent 1 and the control agent 2 described below on the root length and the bud length of cucumber were measured. Wherein the contrast medicament 1 is 15% paclobutrazol wettable powder, and the contrast medicament 2 is 25% paclobutrazol suspending agent.

And determining the influence of the paclobutrazol water emulsion 5, the control medicament 1 and the control medicament 2 on the root length and the bud length of the cucumber by referring to a determination method of a plate herbicide NY/T1155.1-2006.

Dissolving and diluting the paclobutrazol water emulsion 5, the contrast medicament 1 and the contrast medicament 2 by using distilled water, and respectively preparing 100g of mother liquor with four concentrations of 10mg/kg, 25mg/kg, 50mg/kg and 100 mg/kg. Selecting 20 cucumber seeds with the same germination and placing the cucumber seeds in a culture dish (diameter is 9cm) padded with 2 pieces of filter paper, enabling the directions of radicles and germs to be consistent when the cucumber seeds are placed, adding 9 milliliters of liquid medicine with the series of concentrations into the culture dish to soak the seeds, taking clear water as blank control, sealing the treated culture dish by using a preservative film, placing the culture dish into an artificial climate box, culturing the cucumber seeds under the dark condition of the temperature of (25 +/-1) DEG C and the humidity of 80-90 percent, repeating the treatment for not less than four times and setting the treatment without the medicament as the blank control to observe the germination phenomenon, and calculating the inhibition rate of the root length and the bud length of the cucumber.

Inhibition rate of 100 ═ root length (bud length) of control group-root length (bud length) of treated group/root length (bud length) of control group

The significance of the difference was determined using DPS data processing software (version 14.50), and the regression equation was calculated using the log of the drug concentration as the independent variable x and the suppression rate probability as the dependent variable y, and the theoretical EC was calculated₅₀The value is obtained.

The inhibition effect of the paclobutrazol water emulsion 5, the control medicament 1 and the control medicament 2 on the cucumber root length is shown in the table 1 and the table 2, wherein different lower case letters indicate that the level difference of p < 0.05 is obvious.

TABLE 1 inhibition of cucumber root length by different formulations of paclobutrazol

TABLE 2 indoor determination of the activity of paclobutrazol in different formulations on cucumber root length

As can be seen from tables 1 and 2, the EC for cucumber root length of control 2₅₀Maximum value of 109.28mg/kg, followed by control 1, EC₅₀At 16.5611mg/kg, the EC of the paclobutrazol water emulsion 5 provided by the embodiment of the disclosure₅₀Is 12.51mg/kg less than the control medicament 1 and the control medicament 2. Therefore, the paclobutrazol water emulsion 5 provided by the embodiment of the disclosure has better inhibition effect on cucumber root length than the control medicament 1 and the control medicament 2.

The inhibition effect of the paclobutrazol water emulsion 5, the control medicament 1 and the control medicament 2 on cucumber bud length is shown in tables 3 and 4, wherein different lower case letters indicate that the level difference of p < 0.05 is obvious.

TABLE 3 inhibition of cucumber shoot growth by paclobutrazol in different dosage forms

TABLE 4 indoor Activity measurement results of different formulations of paclobutrazol for cucumber bud length

As can be seen from tables 3 and 4, EC of control 1 on cucumber shoot length₅₀Maximum value of 138.03mg/kg, followed by control 2, EC₅₀Is 64.09mg/kg, and the EC of the paclobutrazol water emulsion 5 provided by the embodiment of the disclosure on cucumber bud length₅₀Is 29.02mg/kg less than the control medicament 1 and the control medicament 2. Therefore, the paclobutrazol water emulsion 5 provided by the embodiment of the disclosure has better inhibition effect on cucumber bud growth than the control medicament 1 and the control medicament 2.

The embodiment of the disclosure provides a field efficacy test of paclobutrazol water emulsion on peanut growth.

The paclobutrazol water emulsion 5 is used as a test medicament, and 15% paclobutrazol wettable powder is used as a control medicament 3.

TABLE 5 field application dosage of different formulations of paclobutrazol to peanut treatment

TABLE 6 Effect of different formulations of paclobutrazol on peanut growth and yield

As can be seen from table 6, the paclobutrazol aqueous emulsion 5 provided by the embodiment of the disclosure has a certain promotion effect on the kernel ratio, the weight of the pods and the yield of the peanuts, and has no significant difference from the control medicament 3.

The embodiment of the disclosure provides a field efficacy test of paclobutrazol water emulsion on wheat growth.

TABLE 7 field application dosage of different formulations of paclobutrazol to wheat treatment

TABLE 8 Effect of different formulations of paclobutrazol on wheat growth and yield

The paclobutrazol water emulsion can be applied at the initial stage of wheat jointing, the stem and leaf spraying is carried out, the liquid medicine amount is 450 liters per hectare, the optimal concentration is 100-150 mg/kg of the effective component, the paclobutrazol water emulsion has a good adjusting effect on the growth of wheat plants, the plant growth can be inhibited to a certain degree, the lodging resistance of wheat is enhanced, and the yield increasing effect is obvious. The treatment dosage is safe to wheat and has no phytotoxicity symptom.

In recent years, people pay more and more attention to some low-toxicity and low-residue pesticides, and the national requirements for registration and registration of new pesticide varieties are more and more strict, but due to the limitation of production technology and production scale, the development difficulty of new pesticide varieties is higher, the cost is higher, time and labor are wasted, and the expected effect is not necessarily achieved. In order to solve the problems, the embodiment of the disclosure provides a paclobutrazol aqueous emulsion which has a good growth regulation effect on crops such as cucumbers, is superior to paclobutrazol wettable powder and paclobutrazol suspension concentrate, has low cost, is environment-friendly, is safe for operators, and has certain social and economic benefits.

The ranges of the mass fraction of each component described in the present application include not only two end values of each range, but also all values between the two end values and a range value consisting of any two values between the two end values. For example, the paclobutrazol may be present in an amount of 8 to 12% by mass, where 8 to 12 includes not only the two endpoints 8, 12 but also all values between 8 and 12, and any two values between 8 and 12 (e.g., 10, 11) constituting a range of values (e.g., 10 to 11).

The paclobutrazol aqueous emulsion provided by the application and the preparation method and application thereof are not limited to the examples listed in the above embodiments. The scope of protection of the application is defined by the content of the claims.