CN117814220A - Pesticide dispersible oil suspending agent and preparation method and application thereof - Google Patents

Pesticide dispersible oil suspending agent and preparation method and application thereof Download PDF

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Publication number
CN117814220A
CN117814220A CN202311846438.7A CN202311846438A CN117814220A CN 117814220 A CN117814220 A CN 117814220A CN 202311846438 A CN202311846438 A CN 202311846438A CN 117814220 A CN117814220 A CN 117814220A
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percent
agent
optionally
polyoxyethylene ether
dispersible oil
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李志清
曾庆磊
王建伟
赵保臣
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Shandong Weifang Rainbow Chemical Co Ltd
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Shandong Weifang Rainbow Chemical Co Ltd
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    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02ATECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A50/00TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
    • Y02A50/30Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change

Abstract

The invention discloses a dispersible oil suspending agent, a preparation method and application thereof, and relates to the field of pesticides, wherein the dispersible oil suspending agent comprises the following raw materials in percentage by weight: 5 to 35 percent of atrazine, 5 to 30 percent of dimethyltetracloisonne, 1 to 10 percent of topramezone, 1 to 5 percent of dispersing agent, 5 to 20 percent of emulsifying agent, 1 to 5 percent of rheological agent, 0.1 to 5 percent of stabilizing agent, 0 to 10 percent of other auxiliary agent and 15 to 65 percent of dispersing medium; the dispersing agent comprises at least one of EO/PO block copolymer, phosphate, polyurethane type block copolymer and sulfonate type macromolecular dispersing agent; the emulsifier comprises at least one of castor oil polyoxyethylene ether, fatty alcohol polyoxyethylene ether, oleic acid polyoxyethylene ether, potassium sorbitan monooleate polyoxyethylene ether and calcium dodecyl benzene sulfonate; the stabilizer is an alkaline compound. The invention solves the problems of poor stability and high cost of the dispersible oil suspending agent.

Description

Pesticide dispersible oil suspending agent and preparation method and application thereof
Technical Field
The invention relates to the technical field of pesticides, in particular to a pesticide dispersible oil suspending agent, a preparation method of the pesticide dispersible oil suspending agent, a use method of the pesticide dispersible oil suspending agent and application of the pesticide dispersible oil suspending agent and the pesticide dispersible oil suspending agent in controlling plant insect pests in farmlands.
Background
Atrazine is a systemic selective pre-seedling and post-seedling closed herbicide, the root absorption is dominant, the stem and leaf absorption is little, and the atrazine is rapidly transmitted to plant meristems and leaves to interfere photosynthesis, so that weeds are killed. In resistant crops such as corn, the corn ketolase is decomposed to generate nontoxic substances, so that the corn ketolase is safe to crops;
the dimethyl isooctyl chloride is a selective activator phenoxy carboxylic acid herbicide and has stronger absorption conductivity. The preparation is mainly used for post-emergence stem and leaf treatment, passes through the stratum corneum and cell membranes and finally is conducted to all parts. The action mode is selectively the same as that of 2, 4-D. But the volatility and the action speed of the composition are lower than those of 2, 4-butyl ester emulsifiable concentrate, so that the composition is safer to use than 2, 4-butyl ester emulsifiable concentrate in rice areas in cold regions.
Topramezone is a benzyl ester pyrazolone herbicide, post-emergence stem and leaf treatment is absorbed by roots, seedlings and leaves, is conducted to meristems in a plant to the top and the base, inhibits p-hydroxyphenylpyruvate dioxygenase (4-HPPD), inhibits biosynthesis of carotenoid by plastid quinone and indirectly, has chloroplast synthesis and function disturbance, causes albinism of germinated sensitive weeds due to oxidative degradation of chlorophyll, accompanies growth inhibition, causes tissue necrosis of which the damage symptom is similar to chlorosis under photosynthesis, bleaches the sensitive target weeds within 2-5 days after treatment, and dies plants within 14 days.
Herbicide varieties of a single active ingredient often suffer from varying degrees of deficiencies in agricultural pest control, including but not limited to: the weeding spectrum is narrow, drug resistance is easy to generate after continuous use, and environmental pollution can be aggravated after the use times are more. The active ingredients with different action mechanisms can be compounded to effectively overcome the defects. Meanwhile, the synergistic effect generated by mixing different active components can improve the control effect, expand the weeding spectrum, delay the generation of weed drug resistance and reduce the environmental pollution, thus being an important means for comprehensively preventing and controlling weeds. However, after different effective components are compounded, the product is unstable and even reacts with each other to decompose the effective components because of the physicochemical properties of the effective components such as melting point, solubility, pH value and the like, so that the compounding of the product is required to be optimized and the formula is required to be reasonably matched; the stability of the product can be maintained, and the product has the advantages of high drug effect and the like.
The development of the dispersible oil suspending agent starts from the later 70 s and gradually progresses to the 80 s. Because of the differences in the effectiveness of water-based, granulated products, particularly pharmaceutical effects, in many cases compared to emulsifiable concentrates, dispersible oil suspensions are a desirable option in some cases. The dispersible oil suspending agent can improve the capability of the liquid medicine to permeate the waxy layer and the cuticle of the leaf surface through the use of an oil dispersion medium and the addition of an oil-based system auxiliary agent, so that the liquid medicine can enter the tissue in the leaf more smoothly, and meanwhile, the oil-based system is beneficial to improving the deposition capability, the rainwater washing resistance and the transpiration resistance of the medicament, and the effects can promote the efficacy to play and play an obvious synergistic effect. Despite the above advantages of preparing dispersible oil suspensions, developing a stable, efficient, high content dispersible oil suspension product remains a challenge for formulation engineers. High levels of dispersible oil suspending agent products tend to suffer from high formulation viscosity, poor dispersion, easy settling and bottoming.
But the topramezone is easy to degrade when being prepared into a dispersible oil suspending agent, and is difficult to obtain the dispersible oil suspending agent with good thermal storage stability at 54 ℃ due to the adjustment and change of auxiliary agents when being used together with other herbicides, so that the effective period of the product is short, and the drug effect and the weeding effect of the compound composition are seriously influenced. In view of the fact that the topramezone dispersible oil suspending agent is decomposed under the influence of various factors to reduce the activity and finally influence the pesticide effect, the problem that the effective components are prevented from being decomposed and the stability of the effective components in the process of storage and transportation is maintained is a difficulty in the research of the technical field of pesticides. Therefore, there is an urgent need to find a dispersible oil suspension herbicidal composition containing topramezone with good stability.
Disclosure of Invention
Object of the Invention
In order to overcome the defects, the invention aims to provide a pesticide dispersible oil suspending agent and a preparation method and application thereof.
The invention adopts the compound composition of atrazine, dimethyl isooctyl chloride and topramezone, and the dispersible oil suspending agent is obtained through a large number of screening and experiments, thereby overcoming the defect of poor stability of the traditional dispersible oil suspending agent, greatly reducing the abnormality of separated chromatographic oil during the shelf life or the product transportation and solving the problems of sedimentation and bottoming; and the problem that three effective components are compounded and are easy to decompose is solved by screening the compound stabilizer, so that the physical and chemical stability of the product is greatly increased, and the compound stabilizer has great advantages for long-term storage of customers.
The herbicide (atrazine 25% + dimethyl isooctyl chloride 15% + topramezone 2%) OD of the invention ensures that the herbicide has obvious synergistic effect on the weeding effect of corn fields, greatly delays the generation of weed resistance, and has the advantages of environmental friendliness, high efficacy, no need of barrel mixing auxiliary agent and convenient use; meanwhile, the problems of poor stability and high cost of the dispersible oil suspending agent are solved.
Solution scheme
In order to achieve the purpose of the invention, the technical scheme adopted by the invention is as follows:
in a first aspect, the invention provides a pesticide dispersible oil suspension comprising the following raw materials in percentage by weight: 5 to 35 percent of atrazine, 5 to 30 percent of dimethyltetracloisonne, 1 to 10 percent of topramezone, 1 to 5 percent of dispersing agent, 5 to 20 percent of emulsifying agent, 1 to 5 percent of rheological agent, 0.1 to 5 percent of stabilizing agent, 0 to 10 percent of other auxiliary agent and 15 to 65 percent of dispersing medium;
the emulsifier comprises at least one of castor oil polyoxyethylene ether, fatty alcohol polyoxyethylene ether, oleic acid polyoxyethylene ether, potassium sorbitan monooleate polyoxyethylene ether and calcium dodecyl benzene sulfonate;
the other auxiliary agents comprise zero, one or more of antifreezing agents, defoamers and preservatives.
Further, the stabilizer is an alkaline compound; optionally, the stabilizer is at least one of alkali metal hydroxide, bicarbonate, carbonate and silicate; optionally, the stabilizer is at least one of alkali metal hydroxide, alkali metal bicarbonate, alkali metal carbonate and alkali metal silicate; optionally, the stabilizer is selected from one or more of sodium hydroxide, potassium hydroxide, sodium bicarbonate, potassium bicarbonate, sodium carbonate, potassium carbonate, sodium silicate and potassium silicate; optionally, the stabilizer is selected from one or more of sodium hydroxide, sodium bicarbonate, sodium carbonate and sodium silicate.
Further, the stabilizer comprises 0.3 to 2%, alternatively 0.3 to 1%, alternatively 0.5 to 1% by weight of the dispersible oil suspending agent.
Further, the dispersion medium is selected from at least one of methyl esterified vegetable oil such as methyl oleate, soybean oil methyl ester, rapeseed oil methyl ester; alternatively methyl oleate; optionally, the dispersion medium comprises 17 to 61%, optionally 17 to 38% by weight of the dispersible oil suspending agent.
Further, the rheological agent comprises one or two of organic bentonite and white carbon black, and optionally, the weight ratio of the organic bentonite to the white carbon black is 2: (0-3), optionally 2: (0-1).
Further, the emulsifier comprises calcium dodecyl benzene sulfonate and other ether dispersants, and the other ether dispersants comprise one or more of castor oil polyoxyethylene ether, fatty alcohol polyoxyethylene ether, oleic acid polyoxyethylene ether and potassium sorbitan monooleate polyoxyethylene ether.
Further, the weight ratio of the calcium dodecyl benzene sulfonate and other ether dispersants is (1-5): 12, optionally (2-3.5): 12, optionally (2.5-3.5): 12.
further, the dispersing agent comprises at least one of EO/PO block copolymer, phosphate ester, polyurethane type block copolymer and sulfonate type macromolecule dispersing agent.
Further, the weight ratio of the dispersant, the emulsifier and the dispersion medium is (2-3): (14-15.5):
(17-61), optionally (2-3): (14.5-15.5): (17-38).
Further, the weight ratio of atrazine, dimethyl tetrachlor isooctyl ester and topramezone is (10-35): (8-20):
(2-5), optionally (25-35): (15-20): (2-5).
Further, the material comprises the following raw materials in percentage by weight: 10 to 35 percent of atrazine, 8 to 20 percent of isooctyl methochloride, 2 to 5 percent of topramezone, 2 to 5 percent of dispersing agent, 12 to 18 percent of emulsifying agent, 2 to 5 percent of rheological agent, 0.3 to 2 percent of stabilizing agent, 0 to 10 percent of other auxiliary agent and 17 to 61 percent of dispersing medium.
Further, the material comprises the following raw materials in percentage by weight: 10 to 35 percent of atrazine, 8 to 20 percent of isooctyl dimethyltetrachloride, 2 to 5 percent of topramezone, 2 to 3 percent of dispersing agent, 14 to 15.5 percent of emulsifying agent, 2 to 3 percent of rheological agent, 0.3 to 1 percent of stabilizing agent, 0 to 10 percent of other auxiliary agent and 17 to 61 percent of dispersing medium.
Further, the material comprises the following raw materials in percentage by weight: 25 to 35 percent of atrazine, 15 to 20 percent of isooctyl dimethyltetrachloride, 2 to 5 percent of topramezone, 2 to 3 percent of dispersing agent, 14.5 to 15.5 percent of emulsifying agent, 2 to 3 percent of rheological agent, 0.5 to 1 percent of stabilizing agent, 0 to 10 percent of other auxiliary agent and 17 to 38 percent of dispersing medium.
Further, the material comprises the following raw materials in percentage by weight: 25 to 35 percent of atrazine, 15 to 20 percent of isooctyl dimethyltetrachloride, 2 to 5 percent of topramezone, 2 to 3 percent of dispersing agent, 14.5 to 15.5 percent of emulsifying agent, 2.5 to 3 percent of rheological agent, 0.5 to 1 percent of stabilizing agent, 0 to 10 percent of other auxiliary agent and 17 to 38 percent of dispersing medium.
Further, the material comprises the following raw materials in percentage by weight: 25-30% of atrazine, 15% of dimethyl isooctyl chloride, 2-5% of topramezone, 2-3% of sulfonate polymer dispersant or polyurethane block copolymer, 12% of fatty alcohol polyoxyethylene ether or sorbitan potassium monooleate polyoxyethylene ether, 2.5% of calcium dodecyl benzene sulfonate, 2-2.5% of organic bentonite, 0-1% of white carbon black, 0.5-1% of stabilizer, 0-10% of other auxiliary agents and 17-38% of methyl oleate.
Further, the material comprises the following raw materials in percentage by weight: 25 to 35 percent of atrazine, 15 to 20 percent of dimethyl isooctyl chloride, 2 to 5 percent of topramezone, 2 to 3 percent of sulfonate polymer dispersant or polyurethane block copolymer, 12 percent of fatty alcohol polyoxyethylene ether or sorbitan potassium monooleate polyoxyethylene ether, 2.5 to 3.5 percent of calcium dodecyl benzene sulfonate, 2 to 2.5 percent of organic bentonite, 0 to 1 percent of white carbon black, 0.5 to 1 percent of stabilizer, 0.1 to 5 percent of defoamer and 17 to 38 percent of methyl oleate.
Further, the material comprises the following raw materials in percentage by weight: 25-30% of atrazine, 15% of dimethyl isooctyl chloride, 2-5% of topramezone, 2% of sulfonate polymer dispersant or polyurethane type segmented copolymer, 12% of fatty alcohol polyoxyethylene ether or sorbitan potassium monooleate polyoxyethylene ether, 2.5% of calcium dodecyl benzene sulfonate, 2% of organic bentonite, 1% of white carbon black, 0.5-1% of stabilizer, 0.1-5% of defoamer and 29-38% of methyl oleate.
Further, methyl oleate makes up 100%.
Further, the material comprises the following raw materials in percentage by weight: 25% of atrazine, 15% of isooctyl dimethyl tetrachloride, 2% of topramezone, 2% of sulfonate polymer dispersant or polyurethane block copolymer, 12% of fatty alcohol polyoxyethylene ether or sorbitan potassium monooleate polyoxyethylene ether, 2.5% of calcium dodecyl benzene sulfonate, 2% of organic bentonite, 1% of white carbon black, 0.5-1% of stabilizer, 0.1-5% of defoamer and 100% of methyl oleate.
Further, the other auxiliary agents comprise at least one, two, three or four auxiliary agents in the following weight fractions:
0-5% of antifreezing agent; optionally, the antifreezing agent is one or more of propylene glycol, ethylene glycol and glycerol;
0 to 1% of defoaming agent, optionally 0.1 to 0.5%; the defoaming agent is at least one of a polyether defoaming agent, an organic silicon defoaming agent or a polyether modified polysiloxane defoaming agent;
and 0-5% of preservative, optionally one or more of paraformaldehyde, isothiazolinone and potassium sorbate.
In a second aspect, there is provided a method for preparing the pesticide-dispersible oil suspension agent according to the first aspect, comprising: mixing a dispersion medium and a rheological agent, adding an emulsifier, a dispersing agent, a stabilizing agent and other auxiliary agents into a reaction kettle after full activation, and fully mixing and uniformly dispersing; sequentially adding atrazine, dimethyl tetracloisonne isooctyl ester and topramezone under a high-speed shearing state, and mixing to obtain a stable dispersible oil suspending agent;
optionally, the mixture is milled after mixing to a mixture particle size D90 of less than 5 μm.
In a third aspect, there is provided a method of using the pesticide dispersible oil suspension of the first aspect or the dispersible oil suspension prepared by the method of preparation of the second aspect, the dispersible oil suspension being diluted with water and applied by spraying, optionally at a dilution factor of 300-800.
In a fourth aspect, there is provided a use of the pesticide-dispersible oil suspension of the first aspect or the pesticide-dispersible oil suspension prepared by the preparation method of the second aspect for controlling weeds in cultivated or non-cultivated lands; alternatively, the weeds are annual and perennial weeds in a corn field; optionally, the cultivated or non-cultivated land weeds comprise one or more of foxtail, barnyard grass, acalypha australis, goosegrass, wild oat, green bristlegrass, crabgrass, purslane, quinoa, galium, rape, black nightshade, ragweed, water thorn needle, field bindweed and teff.
Advantageous effects
(1) The compound pesticide composition of atrazine, dimethyl isooctyl chloride and topramezone has higher weeding effect, reduces the dosage of herbicide and the application frequency, thereby reducing the cost of the medicament.
(2) The invention carries out a large amount of screening work on the auxiliary agent system, and finally obtains the system with the best matching degree among the components, especially 3 components of the emulsifier, the dispersant and the rheological agent, thereby greatly reducing the processing difficulty of the dosage form, improving the stability of the dosage form, having the advantages of good emulsifying dispersibility and high suspension rate, effectively solving the problems of sample storage creaming, flocculation, particle size growth and the like, and having excellent physical stability after long-term placement. Through screening the stabilizer, the degradation problem of the obtained product after long-term storage is obviously improved, so that the use effect of the product after long-term storage is still excellent for customers.
(3) The pesticide preparation provided by the invention is safe to corn crops and has good pesticide effect on annual and perennial weeds; the product adopts safe and environment-friendly methyl esterification vegetable oil, is safe to transport and environment-friendly to use.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
In addition, numerous specific details are set forth in the following description in order to provide a better illustration of the invention. It will be understood by those skilled in the art that the present invention may be practiced without some of these specific details. In some embodiments, materials, protocols, methods, means, etc. well known to those skilled in the art are not described in detail in order to highlight the gist of the present invention.
Throughout the specification and claims, unless explicitly stated otherwise, the term "comprise" or variations thereof such as "comprises" or "comprising", etc. will be understood to include the stated element or component without excluding other elements or components.
The weeding composition provides a new choice for weed control. The present disclosure is further illustrated by the following examples, but the present disclosure is not limited thereby.
Atrazine, isooctyl dimethyltetrachloride and topramezone are commercially available in the following examples, and other auxiliary agents are commercially available.
The invention is illustrated in further detail by the following examples.
The inventor finally obtains a system with the best matching degree among the components through a large number of screening works, particularly the screening and the combination of 3 components of an emulsifying agent, a dispersing agent and a dispersing medium, greatly reduces the processing difficulty of the dosage form, improves the stability of the dosage form, has the advantages of good emulsifying and dispersing properties and high suspension rate, effectively solves the problems of sample storage creaming, flocculation, particle size growth and the like, and has excellent physical stability after long-term placement. Through screening the stabilizer, the degradation problem of the obtained product after long-term storage is obviously improved, so that the use effect of the product after long-term storage is still excellent for customers. Specifically, the formulation of some examples is shown in table 1:
table 1 formulations of examples and comparative examples
In the above examples and comparative examples, both the auxiliary and the primary drug are commercially available, for example, the sulfonate-based polymeric dispersant may be an alkyl naphthalene sulfonate formaldehyde polycondensate dispersant, available from Noron or Henschel, the lignin sulfonate dispersant may be available from Maidemansiella pekinensis or Bolich, and the polyurethane-based block copolymer may be available from Jinan Jinhe.
In the above examples and comparative examples, dispersible oil suspensions were prepared as follows: mixing a dispersion medium and a rheological agent, adding an emulsifier, a dispersing agent, a defoaming agent and a stabilizing agent into a reaction kettle after full activation, and fully mixing and uniformly dispersing; sequentially adding atrazine, dimethyl isooctyl chloride and topramezone under a high-speed shearing state, mixing and homogenizing for 10-30 minutes, and then grinding until the particle size D90 of the mixture is smaller than 5 mu m to obtain the stable dispersible oil suspending agent.
The properties of the dispersible oil suspension prepared in the above examples were examined:
test example 1
The suspension rate was measured by the GB/T14825-2006 pesticide suspension rate measurement method, the pourability was measured by the GB/T31737-2015 pesticide pourability measurement method, the dispersion stability was measured by the International pesticide analysis Cooperation Commission CIPAC MT 180 "suspension emulsion dispersion stability measurement", and the pourability was measured by the GB/pesticide pourability measurement method, and the results are shown in Table 2.
TABLE 2 product Properties of the dispersible oil suspensions of examples 1-8 and comparative examples 1-4
As can be seen from the above Table 2, the invention, through screening of the auxiliary agent, especially optimization of the emulsifier, the dispersant and the solvent, significantly improves the physical stability of the product, especially examples 3, 4, 5 and 8.
Test example 2
The above examples were subjected to thermal storage stability analysis, the content of topramezone before and after 14 days of thermal storage at 54℃was detected, the detection of topramezone was carried out by conventional methods such as CIPAC or AOAC, and the degradation rate was calculated, and the results are shown in Table 3.
TABLE 3 stability analysis of topramezone of examples 1 to 8 and comparative examples 1 to 4
From the above table, it can be seen that: the stability of the topramezone is obviously improved through the optimization of the stabilizer.
Field test example 1
Experiment site: the test is arranged in a field suburban in a frigid pavilion area of a city in Shandong province, has flat land, complete irrigation and drainage facilities, consistent field management level and even fertility, and is suitable for the field. Corn is sowed in 2022, 6 and 10 days, the variety is Zhensweet No. six, the cultivation mode is direct seeding, and the main weeds in the test field are crabgrass, barnyard grass, green bristlegrass, acalypha australis, amaranthus retroflexus, chenopodium quinoa and the like.
Experimental conditions: and (5) carrying out stem and leaf spraying treatment on the corn in the 4-5 leaf stage. The pesticide is applied by a worker pesticide-16 knapsack manual sprayer for 1 time, 450kg of water is added according to the dosage of each hectare preparation to prepare the pesticide, and the pesticide is uniformly sprayed according to the amount of the pesticide in a converted district. With random block arrangement, 4 repetitions, cell area 30m 2 . Weather was good during the test period and no rain was present on the day of application.
Experimental grouping: a total of 3 treatments were set up, each: treatment 1: spraying clear water and blank control; treatment 2: examples 3, 4, 7 and comparative example 1; treatment 3: the compositions included a control agent (atrazine 25% + dimethyl isooctyl chloride 15% + topramezone 2%) as a dispersible oil suspension (commercially available sample 1, available from Hebei Zhi Chemie Co., ltd.), (atrazine 25% + topramezone 2%) as a dispersible oil suspension (commercially available sample 2, available from Shandong Hailier chemical Co., ltd.), (atrazine 25% + dimethyl tetrachloro 20%) as a suspension (commercially available sample 3, available from Liaoning Hai Jia Agrochemical Co., ltd.). Each medicament is sprayed on stems and leaves according to the dosage of the active ingredients of 650 g/hectare.
Drug efficacy test observation and data arrangement
The weed fresh weight control efficiency calculating method comprises the following steps:
control effect (%) = (fresh weed weight in control area-fresh weed weight in treated area)/fresh weed weight in control area 100 × fresh weed weight in control area
The investigation method for the fresh weight control effect of weeds comprises the following steps:
30d after application, 4 points are randomly taken from each cell, each point is 0.25m < 2 >, all annual weeds are pulled out to be classified as grass fresh weight, and the fresh weight control effect is calculated, and the result is shown in the following table 4.
Table 4 fresh weight control results of each treatment agent for controlling annual weeds in sweet corn fields
From the above table, the efficacy of example 3 and example 4 is better than that of ordinary example 7, and is significantly better than that of comparative example and the current commercial samples, demonstrating that the auxiliary agent of the present invention can improve the control effect of the active ingredient.
The safety of each treatment against fresh weight of weeds and against corn was investigated. The results are shown in Table 5 below.
The corn safety investigation method comprises the following steps:
and observing whether the pesticide is harmful to corn or not 30d after pesticide application, and recording the type and degree of the pesticide. Grading the phytotoxicity of each cell according to a phytotoxicity grading method: grade 1, normal corn growth, no signs of injury; grade 2, corn with slight phytotoxicity less than 10%; grade 3, the pesticide injury in corn and the like can be recovered later, and the yield is not affected; grade 4, the corn has heavier phytotoxicity, is difficult to recover, and causes yield reduction; grade 5, the corn has serious phytotoxicity and cannot be recovered, resulting in obvious yield reduction or absolute yield.
Table 5 safety of each treatment agent on sweet corn
Experimental grouping Dosage (a.i g/hectare) Grade of phytotoxicity
Example 3 650 1
Example 4 650 1
Example 7 650 1
Comparative example 1 650 3
Commercially available sample 1 650 2
Commercial sample 2 650 1
Commercially available sample 3 650 2
From the above table, examples 3, 4, 7 and commercial sample 2 were superior to the other treatment groups in terms of safety to corn.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention, and are not limiting; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit and scope of the technical solutions of the embodiments of the present invention.

Claims (10)

1. The pesticide dispersible oil suspending agent is characterized by comprising the following raw materials in percentage by weight: 5 to 35 percent of atrazine, 5 to 30 percent of dimethyltetracloisonne, 1 to 10 percent of topramezone, 1 to 5 percent of dispersing agent, 5 to 20 percent of emulsifying agent, 1 to 5 percent of rheological agent, 0.1 to 5 percent of stabilizing agent, 0 to 10 percent of other auxiliary agent and 15 to 65 percent of dispersing medium;
the emulsifier comprises at least one of castor oil polyoxyethylene ether, fatty alcohol polyoxyethylene ether, oleic acid polyoxyethylene ether, potassium sorbitan monooleate polyoxyethylene ether and calcium dodecyl benzene sulfonate;
the other auxiliary agents comprise zero, one or more of antifreezing agents, defoamers and preservatives.
2. The dispersible oil suspension agent of claim 1 wherein the stabilizer is a basic compound; optionally, the stabilizer is at least one of alkali metal hydroxide, bicarbonate, carbonate and silicate; optionally, the stabilizer is at least one of alkali metal hydroxide, alkali metal bicarbonate, alkali metal carbonate and alkali metal silicate; optionally, the stabilizer is selected from one or more of sodium hydroxide, potassium hydroxide, sodium bicarbonate, potassium bicarbonate, sodium carbonate, potassium carbonate, sodium silicate and potassium silicate; optionally, the stabilizer is selected from one or more of sodium hydroxide, sodium bicarbonate, sodium carbonate and sodium silicate;
optionally, the stabilizer comprises 0.3 to 2%, optionally 0.3 to 1%, optionally 0.5 to 1% by weight of the dispersible oil suspending agent.
3. The dispersible oil suspension agent according to claim 1 or 2, characterized in that the dispersing medium is selected from at least one of methyl esterified vegetable oils such as methyl oleate, soybean oil methyl ester, rapeseed oil methyl ester; alternatively methyl oleate; optionally, the dispersion medium accounts for 17-61% of the weight of the dispersible oil suspending agent, and optionally 17-38%;
and/or the rheological agent comprises one or two of organic bentonite and white carbon black, and optionally, the weight ratio of the organic bentonite to the white carbon black is 2: (0-3), optionally 2: (0-1).
4. A dispersible oil suspension according to any one of claims 1 to 3 wherein the emulsifier comprises calcium dodecylbenzene sulfonate and other ether dispersants, the other ether dispersants comprising one or more of castor oil polyoxyethylene ether, fatty alcohol polyoxyethylene ether, oleic polyoxyethylene ether, potassium sorbitan monooleate polyoxyethylene ether; optionally, the weight ratio of the calcium dodecyl benzene sulfonate to the other ether dispersant is (1-5): 12, optionally (2-3.5): 12, optionally (2.5-3.5): 12;
and/or the dispersing agent comprises at least one of EO/PO block copolymer, phosphate, polyurethane type block copolymer and sulfonate type macromolecular dispersing agent.
5. The dispersible oil suspension agent according to any one of claims 1 to 4, wherein the weight ratio of the dispersant, the emulsifier and the dispersing medium is (2 to 3): (14-15.5): (17-61), optionally (2-3): (14.5-15.5): (17-38);
and/or atrazine, dimethyl tetrachlor isooctyl ester and topramezone (10-35): (8-20):
(2-5), optionally (25-35): (15-20): (2-5).
6. The dispersible oil suspension agent according to any one of claims 1 to 5, characterized in that it comprises the following raw materials in weight percentage: 10 to 35 percent of atrazine, 8 to 20 percent of isooctyl methochloride, 2 to 5 percent of topramezone, 2 to 5 percent of dispersing agent, 12 to 18 percent of emulsifying agent, 2 to 5 percent of rheological agent, 0.3 to 2 percent of stabilizing agent, 0 to 10 percent of other auxiliary agent and 17 to 61 percent of dispersing medium;
optionally, the material comprises the following raw materials in percentage by weight: 10 to 35 percent of atrazine, 8 to 20 percent of isooctyl methochloride, 2 to 5 percent of topramezone, 2 to 3 percent of dispersing agent, 14 to 15.5 percent of emulsifying agent, 2 to 3 percent of rheological agent, 0.3 to 1 percent of stabilizing agent, 0 to 10 percent of other auxiliary agent and 17 to 61 percent of dispersing medium;
optionally, the material comprises the following raw materials in percentage by weight: 25 to 35 percent of atrazine, 15 to 20 percent of isooctyl methochloride, 2 to 5 percent of topramezone, 2 to 3 percent of dispersing agent, 14.5 to 15.5 percent of emulsifying agent, 2 to 3 percent of rheological agent, 0.5 to 1 percent of stabilizing agent, 0 to 10 percent of other auxiliary agent and 17 to 38 percent of dispersing medium;
optionally, the material comprises the following raw materials in percentage by weight: 25 to 35 percent of atrazine, 15 to 20 percent of isooctyl methochloride, 2 to 5 percent of topramezone, 2 to 3 percent of dispersing agent, 14.5 to 15.5 percent of emulsifying agent, 2.5 to 3 percent of rheological agent, 0.5 to 1 percent of stabilizing agent, 0 to 10 percent of other auxiliary agent and 17 to 38 percent of dispersing medium;
optionally, the material comprises the following raw materials in percentage by weight: 25-30% of atrazine, 15% of dimethyl isooctyl chloride, 2-5% of topramezone, 2-3% of sulfonate high molecular dispersant or polyurethane block copolymer, 12% of fatty alcohol polyoxyethylene ether or sorbitan potassium monooleate polyoxyethylene ether, 2.5% of calcium dodecyl benzene sulfonate, 2-2.5% of organic bentonite, 0-1% of white carbon black, 0.5-1% of stabilizer, 0-10% of other auxiliary agents and 17-38% of methyl oleate;
optionally, the material comprises the following raw materials in percentage by weight: 25 to 35 percent of atrazine, 15 to 20 percent of dimethyl isooctyl chloride, 2 to 5 percent of topramezone, 2 to 3 percent of sulfonate polymer dispersant or polyurethane block copolymer, 12 percent of fatty alcohol polyoxyethylene ether or sorbitan potassium monooleate polyoxyethylene ether, 2.5 to 3.5 percent of calcium dodecyl benzene sulfonate, 2 to 2.5 percent of organic bentonite, 0 to 1 percent of white carbon black, 0.5 to 1 percent of stabilizer, 0.1 to 5 percent of defoamer and 17 to 38 percent of methyl oleate;
optionally, the material comprises the following raw materials in percentage by weight: 25-30% of atrazine, 15% of dimethyl isooctyl chloride, 2-5% of topramezone, 2% of sulfonate polymer dispersant or polyurethane block copolymer, 12% of fatty alcohol polyoxyethylene ether or sorbitan potassium monooleate polyoxyethylene ether, 2.5% of calcium dodecyl benzene sulfonate, 2% of organic bentonite, 1% of white carbon black, 0.5-1% of stabilizer, 0.1-5% of defoamer and 29-38% of methyl oleate;
alternatively, methyl oleate makes up 100%;
optionally, the material comprises the following raw materials in percentage by weight: 25% of atrazine, 15% of isooctyl dimethyl tetrachloride, 2% of topramezone, 2% of sulfonate polymer dispersant or polyurethane block copolymer, 12% of fatty alcohol polyoxyethylene ether or sorbitan potassium monooleate polyoxyethylene ether, 2.5% of calcium dodecyl benzene sulfonate, 2% of organic bentonite, 1% of white carbon black, 0.5-1% of stabilizer, 0.1-5% of defoamer and 100% of methyl oleate.
7. The dispersible oil suspension agent according to any one of claims 1 to 6, characterized in that the other adjuvants comprise at least one, two, three or four adjuvants in the following weight fractions:
0-5% of antifreezing agent; optionally, the antifreezing agent is one or more of propylene glycol, ethylene glycol and glycerol;
0 to 1% of defoaming agent, optionally 0.1 to 0.5%; the defoaming agent is at least one of a polyether defoaming agent, an organic silicon defoaming agent or a polyether modified polysiloxane defoaming agent;
and 0-5% of preservative, optionally one or more of paraformaldehyde, isothiazolinone and potassium sorbate.
8. A process for the preparation of a pesticide-dispersible oil suspension as claimed in any one of claims 1 to 7, comprising: mixing a dispersion medium and a rheological agent, adding an emulsifier, a dispersing agent, a stabilizing agent and other auxiliary agents into a reaction kettle after full activation, and fully mixing and uniformly dispersing; sequentially adding atrazine, dimethyl tetracloisonne isooctyl ester and topramezone under a high-speed shearing state, and mixing to obtain a stable dispersible oil suspending agent;
optionally, the mixture is milled after mixing to a mixture particle size D90 of less than 5 μm.
9. A method of using the pesticidal dispersible oil suspension of any one of claims 1 to 7 or the dispersible oil suspension prepared by the method of preparation of claim 8, wherein the dispersible oil suspension is diluted with water and applied by spraying, optionally at a dilution factor of 300-800.
10. Use of the pesticide-dispersible oil suspension of any one of claims 1 to 7 or the pesticide-dispersible oil suspension prepared by the preparation method of claim 8 for controlling cultivated or non-cultivated weeds; alternatively, the weeds are annual and perennial weeds in a corn field; optionally, the cultivated or non-cultivated land weeds comprise one or more of foxtail, barnyard grass, acalypha australis, goosegrass, wild oat, green bristlegrass, crabgrass, purslane, quinoa, galium, rape, black nightshade, ragweed, water thorn needle, field bindweed and teff.
CN202311846438.7A 2023-12-28 2023-12-28 Pesticide dispersible oil suspending agent and preparation method and application thereof Pending CN117814220A (en)

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