CN116114703A

CN116114703A - Compound medicine for preventing and treating red rust of mulberry and preparation method thereof

Info

Publication number: CN116114703A
Application number: CN202211446838.4A
Authority: CN
Inventors: 陈俊骥; 朱福新; 周国庆; 杨秋萍; 朱素芹
Original assignee: Jiangsu Shengjiu Agrochemical Co ltd
Current assignee: Jiangsu Shengjiu Agrochemical Co ltd
Priority date: 2022-11-18
Filing date: 2022-11-18
Publication date: 2023-05-16

Abstract

The invention discloses a compound medicament for preventing and treating red rust of mulberry and a preparation method thereof, wherein the compound medicament is prepared from the following raw materials in percentage by weight: 10-25% of tebuconazole technical, 20-40% of prochloraz technical, 15-20% of composite emulsifier, 6-12% of s150 solvent oil, 5-7% of antifreeze agent and stabilizer: 2 to 5 percent, 1 to 3 percent of preservative and 10 to 75 percent of 342mg/L standard hard water. The invention also discloses a preparation method of the compound medicament for preventing and treating the red rust disease of the mulberry. The preparation method is simple and efficient, the tebuconazole and the prochloraz are dissolved in the s150 solvent oil for compounding and mixing, and under the action of the composite emulsifier with high compatibility, the side reaction can be effectively reduced, the stability and the reactivity of the compound medicament are improved, and the prevention and treatment effect of the red rust of the mulberry can be remarkably improved.

Description

Compound medicine for preventing and treating red rust of mulberry and preparation method thereof

Technical Field

The invention relates to the technical field of agricultural science, in particular to a compound medicament for preventing and treating red rust of mulberry and a preparation method thereof.

Background

The rust disease of mulberry is commonly known as golden mulberry, golden leaf, and the like, also known as powdery mildew, and is a fungal disease. The mulberry buds are distributed in all mulberry planting areas nationwide, and are mainly used for damaging the buds, young leaves, young shoots, lattices and the like of the mulberry, and the buds of the mulberry can cause malformation or bending of the diseased part after being damaged by bacteria, so that the buds of the mulberry cannot germinate. After the leaf is stained, round and glossy dots are scattered on the front and back of the leaf, the leaf gradually bulges into a green bubble shape, the color turns yellow (yellow bubble) after the leaf is ripe, the epidermis is broken, orange yellow powdery rust is scattered, and the leaf is fully covered (so the leaf is called as 'Jinsang'). After the rust spores are scattered out, the rust device ages and scorchs into 'scorched bubbles'. The new tip, the leaf stalk and the leaf vein are in longitudinal strip expansion along the vascular bundle direction, bending deformity appears, orange yellow rust devices are generated on the surfaces of the new tip, the disease spots on the new tip are gradually blackened and sunk, and the mulberry flower is in irregular expansion. The mulberry loses the original luster after dying, turns yellow, and is also provided with orange yellow powder in the later stage. Sang Chi rust is serious, which not only causes the yield reduction of mulberry leaves, but also seriously affects the mulberry She Zhiliang, resulting in the apology of cocoons.

At present, the variety of partial mulberry is mixed mainly because the mulberry seedlings are supplied and managed in disorder in the market and lack of strict unified management, and a plurality of inferior mulberry seedlings are sold to farmers through illegal vendors, so that the situation of one garden with more mulberry varieties is caused, and therefore, the Sang Chi rust disease is caused to be infected repeatedly, especially the mulberry varieties which are extremely easy to be infected are planted, the morbidity is far higher than that of the disease-resistant mulberry varieties, so that the disease bacteria are accumulated, remain and further infect, and the income of the farmers is seriously influenced.

However, the existing method for preventing and controlling the red rust disease of the mulberry mainly comprises the steps of selecting a disease-resistant variety, stripping the initially-infected buds, enhancing the management of the mulberry field to prevent moisture retention, spraying medicines and the like, wherein the most common methods are agricultural prevention and control and chemical agent prevention and control, and although the development of the red rust disease of the mulberry can be controlled and relieved through cleaning the field in winter, the method not only needs a large amount of manpower and material resources, has high cost, but also is difficult to thoroughly clean the field, and provides a wintering place for red rust bacteria once a small amount of mulberry branches remain, so that most farmers still mainly adopt chemical agent prevention and control, the traditional chemical agent mainly adopts the powder rust wettable powder, but the chemical agent causes pollution to the environment when being used in a large amount, causes pathogenic bacteria to generate medicine resistance, gradually reduces the medicine effect, and causes certain toxicity to non-target organisms and damages an ecological system. Therefore, there is a need for improvements in the preparation of the above-described chemical agents to enhance the medicinal properties of the chemical agents.

Disclosure of Invention

The invention aims to solve the problems, and provides a compound medicament for preventing and treating mulberry red rust and a preparation method thereof, which are used for improving the prevention and treatment effect of chemical agents, avoiding poisoning non-target organisms, protecting ecological environment and improving the overall medicinal performance.

The technical scheme of the invention is as follows: the compound medicine for preventing and treating the red rust of the mulberry comprises tebuconazole technical, prochloraz technical, compound emulsifier, s150 solvent oil, antifreeze agent, glycol, stabilizer, preservative and 342mg/L standard hard water, and is characterized in that: the coating comprises the following components in percentage by weight: 10-25% of tebuconazole technical, 20-40% of prochloraz technical, 15-20% of composite emulsifier, 6-12% of s150 solvent oil, 5-7% of antifreeze agent and stabilizer: 2 to 5 percent, 1 to 3 percent of preservative and 10 to 75 percent of 342mg/L standard hard water.

Further, the compound medicament for preventing and treating the red rust disease of the mulberry comprises the following components: the antifreeze agent is one of ethylene glycol, propylene glycol, diethylene glycol, ethylene glycol butyl ether, propylene glycol butyl ether, ethylene glycol butyl ether acetate, methylene dichloride, 1-dichloroethane and 1, 2-dichloroethane.

Further, the compound medicament for preventing and treating the red rust disease of the mulberry comprises the following components: the stabilizer is one of dibutyl tin dilaurate, dibutyl tin dimaleate, zinc stearate, cadmium stearate, calcium stearate and zinc stearate.

Further, the compound medicament for preventing and treating the red rust disease of the mulberry comprises the following components: the preservative is one of benzoic acid, sodium benzoate, sorbic acid, sodium sorbate and p-hydroxybenzoic acid.

Further, the compound medicament for preventing and treating the red rust disease of the mulberry comprises the following components: the composite emulsifier is formed by a high molecular emulsifier G-200 and an emulsifier with a multifunctional structure in a ratio of 1.2: 0.85-1.1, wherein the macromolecular emulsifier G-200 is supported by covalent bond crosslinking, and forms a loose three-dimensional network structure in water through intramolecular hydrogen bond and charge action, so that the emulsifier with a multifunctional structure has strong emulsifying action, is a modified functional emulsifier, has excellent thickening and suspending actions, takes 10% cyclohexanone as a compounding auxiliary agent, and ensures that the adaptability of the prepared composite emulsifier is enhanced and the stability of the composite emulsifier is higher than that of a conventional monomer emulsifier under the condition of maintaining optimal pourability.

Further, the compound medicament for preventing and treating the red rust disease of the mulberry comprises the following components: the emulsifier with the multifunctional structure takes tristyrene phenol polyoxyethylene ether, 1, 3-butadiene or cyclopropene and oleic acid as reaction raw materials, and sodium bisulfate as a catalyst, and the preparation method comprises the following steps: under the catalysis of sodium bisulfate, the esterification reaction of the tristyrene phenol polyoxyethylene ether and oleic acid is carried out, and the n (oleic acid) of the tristyrene phenol polyoxyethylene ether and the oleic acid is that: the ratio of n (ether) is 1:1, the dosage of sodium bisulfate accounts for 0.45 percent of the total mass of the trisstyrol polyoxyethylene ether and the oleic acid, sodium bisulfate can be recycled by a reflux method, and the sodium bisulfate continuously reacts for 5 to 6 hours at 130 ℃ to obtain the trisstyrol polyoxyethylene ether oleate; and after the tristyrene phenol polyoxyethylene ether oleate is synthesized, mixing 1, 3-butadiene or cyclopropene, heating in a sealing way, starting stirring to perform full reaction, reacting for 3-5 h, cooling, stopping stirring, standing and layering for 1h to obtain upper-layer slightly turbid flowable liquid, namely the emulsifier with a multifunctional structure.

The invention also provides a preparation method of the compound medicament for preventing and treating the red rust disease of the mulberry, which comprises the following steps:

(1) And mixing and soaking the tebuconazole technical, the prochloraz technical and the s150 solvent oil, and slowly stirring until the tebuconazole technical and the prochloraz technical are dissolved to obtain a uniform mixture.

(2) And (3) adding the composite emulsifier into the mixture dissolved in the step (1), and uniformly stirring to serve as an oil phase for standby.

(3) And then the composite emulsifier is fully stirred and dispersed in 342mg/L standard hard water to prepare a dispersion liquid.

(4) Mixing a stabilizer and a preservative, adding the mixture into the dispersion liquid obtained in the step (3), continuously stirring until the mixture is fully dispersed, and adding an antifreeze agent to prepare a uniform water phase for standby.

(5) Slowly adding the oil phase in the step (2) into the water phase in the step (4) under stirring, continuously stirring for 20min after emulsification, shearing for 10min at high speed, and standing for 1h to form stable emulsion to obtain a compound medicament finished product.

Further, the preparation method of the compound medicament for preventing and treating the red rust disease of the mulberry comprises the following steps: in the step (2), the reaction temperature is 70-90 ℃ and the reaction time is 2-4 hours.

Further, the preparation method of the compound medicament for preventing and treating the red rust disease of the mulberry comprises the following steps: in the step (3), the reaction temperature is 100-120 ℃ and the reaction time is 1-2 hours.

Still further, the preparation method of the compound medicament for preventing and treating the red rust disease of the mulberry comprises the following steps: in the step (5), the stirring speed is more than 300r/min, and the high-speed shearing rotating speed is 5000r/min.

Therefore, by adopting the technical scheme of the invention, the compound preparation has the control effect on the red rust disease of the mulberry, can not influence the mulberry, can not poison non-target organisms, and can be used for controlling the red rust disease of the mulberry.

Compared with the prior art, after the technical scheme is adopted, on the basis of the compounding of the tebuconazole and the prochloraz, the compound emulsifier prepared from the high molecular emulsifier G-200 and the emulsifier with a multifunctional structure can effectively improve the reaction activity and stability of the distributed medicament, so that the compound emulsifier has a better sterilization effect.

Detailed Description

In order to clearly illustrate the technical features and effects of the present invention, the technical scheme of the present invention is further described in detail below so that it is easier to understand and grasp. The following description is presented to enable one of ordinary skill in the art to make and use the invention. The preferred embodiments in the following description are by way of example only and other obvious variations will occur to those skilled in the art.

Wherein, the raw materials used in the invention are all sold in the market or self-prepared.

Example 1

(1) The tebuconazole original drug (chemical name: S) -1-p-chlorophenyl-4, 4-dimethyl-3 (1H-1, 2, 4-triazole-1-methyl) amyl alcohol), the prochloraz original drug (chemical name: N-propyl-N- [ alpha- (2, 4, 6-trichlorophenoxy) -1H-imidazole-1-formamide) and s150 solvent oil are mixed and soaked, and are slowly stirred until dissolved, so that a uniform mixture is obtained.

(2) The composite emulsifier is prepared by mixing a high molecular emulsifier G-200 and an emulsifier with a multifunctional structure according to the ratio of 1.2: mixing the components in a proportion of 0.85, adding the composite emulsifier into the mixture dissolved in the step (1), and uniformly stirring to serve as an oil phase for standby.

(4) And (3) mixing dibutyl tin dilaurate with sodium benzoate, adding the dispersion liquid obtained in the step (3), continuously stirring until the mixture is fully dispersed, and adding propylene glycol to prepare a uniform water phase for later use.

(5) And (3) slowly adding the oil phase in the step (3) into the water phase in the step (4) under stirring at the reaction temperature of 70 ℃ for 2 hours, continuously stirring for 20min after emulsification, shearing for 10min at a high speed, and standing for 1h to form stable emulsion to obtain a finished product of the compound medicament.

Example 2

(2) The composite emulsifier adopts a macromolecular emulsifier G-200 and an emulsifier with a multifunctional structure in a ratio of 1.2: mixing the components in a proportion of 0.95, adding the composite emulsifier into the mixture dissolved in the step (1), and uniformly stirring to serve as an oil phase for standby.

(4) And (3) mixing cadmium stearate and p-hydroxybenzoic acid, adding the dispersion liquid obtained in the step (3), continuously stirring until the dispersion liquid is fully dispersed, and adding ethylene glycol butyl ether to prepare a uniform water phase for standby.

(5) And (3) slowly adding the oil phase in the step (2) into the water phase in the step (4) under stirring, continuously stirring for 20min after emulsification, shearing for 10min at a high speed, and standing for 1h to form stable emulsion to obtain a compound medicament finished product.

Example 3

(4) And (3) mixing dibutyl tin dimaleate and benzoic acid, adding the mixture into the dispersion liquid obtained in the step (3), continuously stirring until the mixture is fully dispersed, and adding propylene glycol butyl ether to prepare a uniform water phase for later use.

(5) And (3) slowly adding the oil phase in the step (2) into the water phase in the step (4) under stirring at 90 ℃ for 4 hours, continuously stirring for 20min after emulsification, shearing for 10min at a high speed, and standing for 1h to form stable emulsion to obtain a compound medicament finished product.

Comparative example 1

430 g/l tebuconazole suspension (purchased from Shandong Bainongda Biotechnology Co., ltd.).

Comparative example 2

450 g/l prochloraz aqueous emulsion (purchased from Hebei province pesticide chemical Co., ltd.).

Comparative example 3

Clear water (CK).

According to the technical scheme of the invention, a foliar spray method is used for applying the pesticide, the mulberry leaves are uniformly applied, the leaves are fully wetted and do not drip water as a balance measure, 2 times of test pesticide application are implemented, 7 days are spaced in the period, the corresponding test crops are mulberry trees, the variety is 'osmanthus Sang You-12', the planting density is 20 cm and 80 cm, 6000 plants (divided into areas) are planted per mu, the soil type of the mu land is loam, the irrigation and drainage are good, and the pH value is 6.8; the weather conditions are as follows: the first medicine application day is cloudy, the southeast wind is level 2 during the medicine application period, and the average temperature is 29.5 ℃; the second time of application (7 days later) is negative, the southeast wind is level 3 during the period of application, and the average temperature is 30.6 ℃; the rainfall days in the whole test period are 7 days, the total rainfall is 38.6mm, the relative humidity is 61-88%, the minimum temperature is 22.2 ℃, the maximum temperature is 37 ℃, and the daily average temperature is 26.2-30.8 ℃.

The specific experimental operation steps are as follows:

(1) The cell dosage of the weighing chamber (BRAND D-1000 pipette number: Y2020023) was 1.1 times that of the medicine.

(2) The pH of the diluent (or water) was measured and recorded with an acidometer (pH-100 portable acidometer, number S2018006): taking down the electrode protective cap of the acidometer, stirring the PH compound electrode in purified water or distilled water, fully cleaning and spin-drying; starting up; immersing the electrode into the measured solution, standing until the PH number is stable, and reading; after the measurement is finished, the device is shut down, cleaned by purified water or distilled water, and covered by an electrode protective cap, the test is carried out for 2 times, and the PH value of the water measured each time is 7.02 and 7.05 respectively.

(3) Adding clear water according to 15-20% of the volume of the sprayer (the sprayer is cleaned before, during and after the application of the medicine), shaking and cleaning the medicine box for 3 times, and finally adding 2-3 liters of clear water, and washing the spray pipe, the spray rod and the spray nozzle.

(4) The sprayer 1L water spraying time(s) was measured 3 times, and the average was taken, and the flow rate measurement result of the sprayer in this test was 55s/L, so that the cell time was converted to 89s, which corresponds to 3.71L of the liquid medicine.

(5) The sprayer is filled with the supernatant water in an amount which is 1.1 times of the water consumption of the cell, and the medicine is pre-sprayed for 3 times clockwise in a blank control area according to the medicine application time of the cell, and the average pace is correspondingly recorded.

(6) The preparation is carried out according to the test treatment number sequence, the actual dosage is 3.71L (more than 10 percent), and the method comprises the following steps: firstly, adding 1L of water into a sprayer, adding pesticide, washing residual pesticide in a pesticide container or a pipette into the sprayer by using a small amount of water, then supplementing the water, covering a cover of the sprayer, shaking the sprayer for 6 times to completely dissolve or uniformly disperse the pesticide liquid, and completing the dispensing.

(7) When the cells are used for spraying the uniform stems and leaves, the actual spraying time and the measured time deviation of the sprayer during calibration cannot exceed 10%, the cells cannot be leaked and re-sprayed, and when the marginal application of the cells is carried out, mist flows are directed to the inside of the cells so as to prevent the influence on surrounding cells.

(8) The highest and lowest temperature and humidity values during administration were recorded using a TH10R hygrothermograph (number: W2018005).

(9) The wind direction and wind speed during the recording test were measured with an IBS-F10 hand-held anemometer (number F2018012) using the following methods: the anemometer is fixedly installed after being placed at a ventilation place which is 100cm higher than the ground, the azimuth direction of the anemometer is adjusted to be consistent with the actual azimuth, and an anemometer switch is turned on to record the wind direction and the wind speed during the test.

And (3) calculating results:

1)

2)

after the control effect data is converted by the square root of the arcsine, the variance analysis is carried out by a Duncan's new complex polar difference method, and different large letters and small letters respectively represent the difference significance to reach the level of 1% and 5%.

Table 1: comparative examples and comparative examples physical properties table

From table 1: the composition has a certain control effect on the red rust disease of the mulberry tree in the test dosage range, is safe to the mulberry tree, has no obvious adverse effect on other organisms, and can be used for controlling the red rust disease of the mulberry tree.

3) 2 plants are surveyed in each district, 5 points in the north and south of the east and west of each mulberry are surveyed, 2 branches are surveyed in each point, the total leaf numbers on two branches are recorded, the leaf numbers of each stage are as follows:

level 0: no symptoms;

stage 1: the area of the disease spots accounts for less than 5% of the whole blade area;

2 stages: the area of the disease spots accounts for 5-20% of the whole leaf area;

3 stages: the area of the disease spots accounts for 21-40% of the whole leaf area;

4 stages: the area of the disease spots accounts for more than 40% of the whole leaf area.

Side effects are observed: the effect on non-target organisms was recorded.

Table 2: comparative examples and comparative table of field efficacy test results of examples for controlling red rust disease of mulberry

From table 2: investigation of control effect 11 days after last administration: the average disease index of the treatment areas of the examples and the control example is between 0.89 and 1.59, and the average disease index of the treatment area of the control example 3 is 5.07. The 2500-fold, 2000-fold and 1500-fold treatment control effects of examples 1 to 3 were: 68.55%, 75.05%, 82.33%; the control effect of the treatment of 2000 times of the control example 1 and 1000 times of the control example 2 was 73.24% and 71.34%. The control effect of 1500 times treatment in examples 1 to 3 is best, which is significantly higher than that of other test agents, and the difference is 1%. The treatment prevention effect is obviously different from that of the treatment of 2000 times of the treatment prevention effect of the control example 1 and 1000 times of the treatment prevention effect of the control example 2, and the difference is 1% obvious level; in addition, through field observation: at the test dose, the continuous medication has no phytotoxicity symptoms on silkworm mulberry in each treatment area, and no harmful effect on other non-target organisms is found.

In the technical scheme of the invention, the added composite emulsifier is a technical key of the invention, and the composite emulsifier improves the reactivity and stability of the tebuconazole and prochloraz compound medicament, so that the effect of preventing and treating the silkworm mulberry rust is better, and the sterilization efficiency is effectively improved.

Compared with the prior art, the technical scheme of the invention has the advantages that the composite emulsifier prepared by using the high molecular emulsifier G-200 and the emulsifier with the multifunctional structure can effectively improve the reactivity and stability of the distribution medicament on the basis of the compounding of the tebuconazole and the prochloraz, so that the composite emulsifier has better sterilization effect, does not influence the mulberry, does not poison non-target organisms, and can be used for preventing and treating the red rust of the mulberry.

The technical scheme, the working process and the implementation effect of the invention are described in detail, and it is to be noted that the description is only a typical example of the invention, and besides, the invention can also have other various specific embodiments, and all the technical schemes formed by adopting equivalent substitution or equivalent transformation fall within the scope of the invention claimed.

Claims

1. The compound medicament for preventing and treating the red rust of the mulberry comprises tebuconazole, prochloraz, a compound emulsifier, s150 solvent oil, an antifreeze agent, a stabilizer, a preservative and 342mg/L standard hard water, and is characterized by comprising the following components in percentage by weight:

tebuconazole prodrug: 10% -25%;

prochloraz as the active ingredient: 20% -40%;

composite emulsifier: 15% -20%;

s150 solvent oil: 6% -12%;

antifreeze agent: 5% -7%;

stabilizing agent: 2% -5%;

preservative: 1% -3%;

342mg/L standard hard water: 10% -75%.

2. The compound medicament for preventing and treating red rust of mulberry as claimed in claim 1, wherein: the composite emulsifier is formed by a high molecular emulsifier G-200 and an emulsifier with a multifunctional structure in a ratio of 1.2: mixing the components according to the proportion of 0.85 to 1.1.

3. The compound medicament for preventing and treating red rust of mulberry as claimed in claim 2, wherein: the emulsifier with the multifunctional structure takes tristyrene phenol polyoxyethylene ether, 1, 3-butadiene or cyclopropene and oleic acid as reaction raw materials, and sodium bisulfate as a catalyst, and the preparation method comprises the following steps: under the catalysis of sodium bisulfate, the esterification reaction of the trisstyrol polyoxyethylene ether and oleic acid is carried out, after the trisstyrol polyoxyethylene ether oleate is synthesized, 1, 3-butadiene or cyclopropene is mixed, the temperature is raised in a sealing way, stirring is started for full reaction, the reaction is carried out for 3-5 hours, after cooling, stirring is stopped, and standing and layering are carried out for 1 hour.

4. The compound medicament for preventing and treating red rust of mulberry as claimed in claim 1, wherein: the antifreeze agent is one of ethylene glycol, propylene glycol, diethylene glycol, ethylene glycol butyl ether, propylene glycol butyl ether, ethylene glycol butyl ether acetate, methylene dichloride, 1-dichloroethane and 1, 2-dichloroethane.

5. The compound medicament for preventing and treating red rust of mulberry as claimed in claim 1, wherein: the stabilizer is one of dibutyl tin dilaurate, dibutyl tin dimaleate, zinc stearate, cadmium stearate, calcium stearate and zinc stearate.

6. The compound medicament for preventing and treating red rust of mulberry as claimed in claim 1, wherein: the preservative is one of benzoic acid, sodium benzoate, sorbic acid, sodium sorbate and p-hydroxybenzoic acid.

7. A method for preparing a compound medicament for preventing and treating red rust of mulberry according to any one of claims 1 to 6, characterized by comprising the steps of:

step S1: mixing and soaking tebuconazole technical, prochloraz technical and s150 solvent oil, and slowly stirring until the tebuconazole technical and prochloraz technical are dissolved to obtain a uniform mixture;

step S2: adding the composite emulsifier into the mixture dissolved in the step S1, and uniformly stirring to serve as an oil phase for standby;

step S3: fully stirring and dispersing the composite emulsifier in 342mg/L standard hard water to prepare a dispersion liquid;

step S4: mixing a stabilizer and a preservative, adding the mixture into the dispersion liquid obtained in the step S3, continuously stirring until the mixture is fully dispersed, and adding an antifreeze agent to prepare a uniform water phase for later use;

step S5: slowly adding the oil phase in the step S2 into the water phase in the step S4 under stirring, continuously stirring for 20min after emulsification, shearing for 10min at high speed, and standing for 1h to form stable emulsion to obtain a compound medicament finished product.

8. The method for preparing the compound medicament for preventing and treating the red rust disease of the mulberry, which is characterized by comprising the following steps of: in the step S2, the reaction temperature is 70-90 ℃ and the reaction time is 2-4 hours.

9. The method for preparing the compound medicament for preventing and treating the red rust disease of the mulberry, which is characterized by comprising the following steps of: in the step S3, the reaction temperature is 100-120 ℃ and the reaction time is 1-2 hours.

10. The method for preparing the compound medicament for preventing and treating the red rust disease of the mulberry, which is characterized by comprising the following steps of: in the step S5, the stirring speed is more than 300r/min, and the high-speed shearing rotating speed is 5000r/min.