CN115211428A - Fluopicolide/dimethomorph composition as well as preparation method and application thereof - Google Patents

Fluopicolide/dimethomorph composition as well as preparation method and application thereof Download PDF

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Publication number
CN115211428A
CN115211428A CN202111076326.9A CN202111076326A CN115211428A CN 115211428 A CN115211428 A CN 115211428A CN 202111076326 A CN202111076326 A CN 202111076326A CN 115211428 A CN115211428 A CN 115211428A
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fluopicolide
dimethomorph
copolymer
ammonium sulfate
composition
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CN115211428B (en
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孟凡睿
周鹏
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Shandong Tongfang Biotechnology Co ltd
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Shandong Tongfang Biotechnology Co ltd
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    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N43/00Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/34Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom
    • A01N43/40Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom six-membered rings
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N37/00Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids
    • A01N37/36Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids containing at least one carboxylic group or a thio analogue, or a derivative thereof, and a singly bound oxygen or sulfur atom attached to the same carbon skeleton, this oxygen or sulfur atom not being a member of a carboxylic group or of a thio analogue, or of a derivative thereof, e.g. hydroxy-carboxylic acids
    • A01N37/38Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids containing at least one carboxylic group or a thio analogue, or a derivative thereof, and a singly bound oxygen or sulfur atom attached to the same carbon skeleton, this oxygen or sulfur atom not being a member of a carboxylic group or of a thio analogue, or of a derivative thereof, e.g. hydroxy-carboxylic acids having at least one oxygen or sulfur atom attached to an aromatic ring system

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Abstract

The invention belongs to the technical field of A01N, and particularly relates to a fluopicolide-dimethomorph composition, and a preparation method and application thereof. The invention provides a fluopicolide-dimethomorph composition, which is prepared from the following raw materials: fluopicolide and dimethomorph; the weight ratio of fluopicolide to dimethomorph is 1: (1-5). According to the fluopicolide-dimethomorph composition provided by the invention, the ethylene oxide propylene oxide copolymer, the acrylic acid crotonic acid copolymer and the polyoxyethylene ether ammonium sulfate salt are added, so that the compatibility of substances in the composition is greatly improved; when the suspending agent is prepared, the heat storage stability of the suspending agent can be ensured, the stability of the suspending agent in the storage process is improved, and the requirement of long-term storage is met; the fluopicolide-dimethomorph composition provided by the invention can control the shear viscosity of a system on the premise of improving the activity of fluopicolide and dimethomorph, and ensures that the suspension stability of the composition reaches more than 99%.

Description

Fluopicolide/dimethomorph composition as well as preparation method and application thereof
Technical Field
The invention belongs to the technical field of A01N pesticides, and particularly relates to a fluopicolide-dimethomorph composition, and a preparation method and application thereof.
Background
The large-scale growth and poor conditions of crops in the planting period are very important reasons for influencing the income of growers. Especially, downy mildew, a plant disease caused by downy mildew among fungi, is spread by air flow or rain, or by means of vectors, insects or people, which causes a wider spread of the spread and increases the damage strength to plants, and therefore, the development of a drug for solving downy mildew of plants is an urgent problem at present.
The Chinese invention patent with the application number of 200910023009.3 discloses a sterilization composition containing fluopicolide and dimethomorph, wherein the disclosed patent ensures that the prepared composition has better effects on the prevention and treatment of cucumber downy mildew, grape downy mildew, tomato late blight and pepper phytophthora blight by changing the proportion of active ingredients of the fluopicolide and the dimethomorph and the synergistic action of a wetting dispersant, a stabilizer, a penetrating agent, an antifreezing agent, a thickening agent and an antifoaming agent. However, the weight ratio of fluopicolide to dimethomorph disclosed in the published patent is in the range of 1:5 or even 5:1 and greater, it is less effective in controlling downy mildew of different soil types.
Therefore, the preparation of the medicine with better control effect on downy mildew is an important measure for solving the problem of crop yield reduction.
Disclosure of Invention
In order to solve the above technical problems, a first aspect of the present invention provides a fluopicolide-dimethomorph composition, which is prepared from the following raw materials: fluopicolide and dimethomorph; the weight ratio of fluopicolide to dimethomorph is 1: (1-5).
In some preferred embodiments, the weight ratio of fluopicolide to dimethomorph is 1: (2-4).
Further preferably, the weight ratio of the fluopicolide to the dimethomorph is 1:3.
in the experimental process, the applicant discovers through a large number of creative experiments that when fluopicolide and dimethomorph are used as active ingredients for controlling downy mildew in the system, the fluopicolide and dimethomorph have better effects on controlling cucumber downy mildew, and particularly have better effects on controlling cucumber downy mildew planted in soil in which other crops are sown within 1 year, and the weight ratio of the fluopicolide to the dimethomorph is controlled to be 1:3, the cucumber downy mildew disease can be guaranteed to be controlled below 4.7, and the applicant speculates that the reason for the phenomenon is that: the fluopicolide has excellent system conductivity and thin layer penetrating power in the system, and can quickly bring the dimethomorph with systemic property into the inner layer of the plant, and the dimethomorph can be transmitted in each part of the plant due to the better systemic action of the dimethomorph, and the penetration of the dimethomorph in the cell wall can be promoted under the weight ratio, so that the control effect of the fluopicolide on the downy mildew can be enhanced.
In addition, for the soil in which other crops are sown within one year, inorganic salt or fertility remained in the soil can be better absorbed by the cucumbers, and medicines possibly remaining in the soil can generate competitive stimulation on fluopicolide and dimethomorph to promote the action effect of the fluopicolide and the dimethomorph, so that the control efficiency reaches 80.3-84.5% after 7 days, the disease index is controlled to be below 4.7, the damage of cucumber downy mildew is reduced, and the control effect is better. And, when the weight ratio of fluopicolide to dimethomorph is 1:3, the applicant found that the efficacy of the composition prepared was not affected by rain.
In some preferred embodiments, the preparation feedstock further comprises at least one of an alkane oxy-derivative copolymer, a carboxylic acid-containing copolymer, a sulfate, an ammonium sulfate salt, and a sulfonate.
In some preferred embodiments, the preparation raw material further comprises alkane oxygen-containing derivative copolymer, carboxylic acid-containing copolymer and ammonium sulfate salt.
In some preferred embodiments, the alkane oxy derivative copolymer comprises at least one of an ethylene oxide propylene oxide copolymer and an ethylene oxide butylene oxide copolymer.
Further preferably, the alkane oxygen-containing derivative copolymer is an ethylene oxide-propylene oxide copolymer.
Ethylene oxide propylene oxide copolymer, available from Jiangsu, qingyu chemical technology, inc.
In some preferred embodiments, the carboxylic acid-containing copolymer comprises at least one of acrylic crotonic acid copolymer, acrylic methacrylic acid copolymer, and polyacrylic acid.
Further preferably, the carboxylic acid-containing copolymer is acrylic butenoic acid copolymer.
Acrylic acid butenoic acid copolymer, available from Jiangsu Qingyu chemical technology Co., ltd.
In some preferred embodiments, the ammonium sulfate salt includes at least one of polyoxyethylene ether ammonium sulfate salt and dodecyl ammonium sulfate salt.
Further preferably, the ammonium sulfate salt is polyoxyethylene ether ammonium sulfate salt.
Polyoxyethylene Ether ammonium sulfate, commercially available from Nanjing Taihua chemical Co., ltd.
In some preferred embodiments, the weight ratio of the ethylene oxide-propylene oxide copolymer, the acrylic acid-crotonic acid copolymer and the polyoxyethylene ether ammonium sulfate salt is (1-5): (1-3): 1.
more preferably, the weight ratio of the ethylene oxide propylene oxide copolymer to the acrylic acid crotonic acid copolymer to the polyoxyethylene ether ammonium sulfate salt is 3:2:1.
during the experiment, the applicant has been researched and researched through a large number of creative experiments, and found that in the application, the control of the types and weight ratios of the ethylene oxide propylene oxide copolymer, the acrylic crotonic acid copolymer and the polyoxyethylene ether ammonium sulfate salt has a great influence on the prepared fluopicolide-dimethomorph composition, especially the suspending agent, and the weight ratio of the ethylene oxide propylene oxide copolymer, the acrylic crotonic acid copolymer and the polyoxyethylene ether ammonium sulfate salt is (1-5): (1-3): 1, which has a large influence on the compatibility of the substances between the compositions and the heat storage stability of the suspending agent, the applicant speculates that this may occur because: the prepared composition, particularly in the form of a suspending agent, can be ionized in a system, so that electronegative particles and electropositive particles exist in the system, and fluopicolide and dimethomorph in the system can be adsorbed on the surfaces of ethylene oxide propylene oxide copolymer, acrylic crotonic acid copolymer and polyoxyethylene ether ammonium sulfate salt, so that substances with more opposite charges can be adsorbed on the surfaces of fluopicolide and dimethomorph, the electrostatic repulsion among ethylene oxide propylene oxide copolymer, acrylic crotonic acid copolymer and polyoxyethylene ether ammonium sulfate salt in the system is increased, and the compatibility and the stability among the substances are improved.
In addition, the fluopicolide-dimethomorph can cause the phenomenon of crystal growth along with the change of temperature or storage conditions in the using or storing process, thereby influencing the using effect of the fluopicolide-dimethomorph as a suspending agent.
In some preferred embodiments, the preparation feedstock further comprises magnesium aluminum silicate.
Further preferably, the particle size of the magnesium aluminum silicate is 300-5000nm.
Further preferably, the particle size of the magnesium aluminum silicate is 300-2000nm.
Further preferably, the particle size of the magnesium aluminum silicate is 1000nm.
Magnesium aluminum silicate, available from new dilute metallurgy chemical company, ltd, guangzhou.
In the experimental process, the applicant finds that the stability of the prepared suspending agent is greatly influenced by adding the magnesium aluminum silicate into the system, and particularly the influence effects of the magnesium aluminum silicate are greatly different when the particle sizes of the magnesium aluminum silicate are different, in the application, the applicant finds through experimental research that the particle size of the added magnesium aluminum silicate is controlled to be 500nm and 1000nm, the shear viscosity of the system can be controlled to be 200-400mPa & s on the premise of improving the activity of the fluopicolide and the dimethomorph, the suspension stability of the system is ensured to be more than 99%, the phenomena such as flocculation, agglomeration and the like are avoided, and the applicant speculates that the possible reasons are that the phenomena occur are that: the particle size of magnesium aluminum silicate added into the system is less than 1000nm, the surface of the magnesium aluminum silicate has higher chemical activity, and when the magnesium aluminum silicate exists in the system, the collision frequency among free particles in the system is increased, so that the agglomeration phenomenon is generated; however, when the particle size of the added magnesium aluminum silicate is larger than 1000nm, the magnesium aluminum silicate is partially dispersed in the ethylene oxide propylene oxide copolymer, the acrylic acid crotonic acid copolymer and the polyoxyethylene ether ammonium sulfate salt, so that the dispersion effect is poor, the system is unstable, the gravity coagulation phenomenon occurs, and the fluopicolide and the dimethomorph are coagulated, so that the drug effect is influenced.
In some preferred embodiments, the weight of the magnesium aluminum silicate is 5-20wt% of the total weight of the oxygen derivative copolymer, the carboxylic acid-containing copolymer and the ammonium sulfate salt.
Further preferably, the weight of the magnesium aluminum silicate is 10wt% of the total weight of the oxygen derivative copolymer, the carboxylic acid-containing copolymer and the ammonium sulfate salt.
In the experimental process, the applicant finds that the existence of the oxygen derivative copolymer, the carboxylic acid-containing copolymer and the ammonium sulfate salt can form better adsorption on the surface of an active substance of fluopicolide and dimethomorph, but when the content of the added magnesium-aluminum silicate is too high, the defoaming property of a system is deteriorated, the active ingredient of fluopicolide and dimethomorph is unstable in a suspending agent, different contact metering at different time can be caused during application, and the phenomenon that the control effects of different crops in the same field are not uniform can be caused; however, if the content of the added magnesium aluminum silicate in the system is reduced and is less than 10wt% of the total weight of the oxygen derivative copolymer, the carboxylic acid-containing copolymer and the ammonium sulfate salt, the thixotropy of the suspending agent is reduced, so that the suspending agent needs to be fully mixed during use, and the requirement on the application link is stricter.
In some preferred embodiments, the preparation raw materials further comprise a thickening agent, an antifoaming agent, a dispersion medium and an antifreezing agent.
In some preferred embodiments, the preparation raw material further comprises white carbon black, and the weight ratio of the white carbon black to the magnesium aluminum silicate is 1: (0.5-2).
Further preferably, the weight ratio of the white carbon black to the magnesium aluminum silicate is 1:1.
in some preferred embodiments, the thickener is not particularly limited as long as the thickening effect in the suspending agent can be achieved.
As a preferred technical scheme, the thickening agent is xanthan gum.
In some preferred embodiments, the antifreeze agent is ethylene glycol.
In some preferred embodiments, the defoamer is a silicone defoamer.
In some preferred embodiments, the preparation raw materials further comprise a preservative and a pH regulator.
As a preferred scheme, the preservative is sodium benzoate.
In a preferred embodiment, the pH regulator is citric acid.
In some preferred embodiments, the weight ratio of the defoamer to the thickener is 1: (0.1-1).
Further preferably, the weight ratio of the defoaming agent to the thickening agent is 1:0.5.
in some preferred embodiments, the dispersion medium is water.
In some preferred embodiments, the preparation raw materials comprise, in weight percent: 5-15% of fluopicolide, 20-35% of dimethomorph, 1-5% of alkane oxygen-containing derivative copolymer, 1-3% of carboxylic acid-containing copolymer, 0.5-2% of ammonium sulfate salt, 0.3-1% of magnesium aluminum silicate, 0.3-1% of white carbon black, 2-5% of antifreezing agent, 0.1-0.5% of preservative, 0.05-0.5% of thickening agent, 0.05-0.2% of pH regulator, 0.1-0.5% of defoaming agent and the balance of dispersion medium being 100%.
The second aspect of the invention provides a preparation method of a fluopicolide-dimethomorph composition, which comprises the following steps:
1) Adding fluopicolide, dimethomorph, alkane oxygen-containing derivative copolymer, carboxylic acid-containing copolymer, ammonium sulfate salt, magnesium aluminum silicate, a thickening agent, a defoaming agent and an antifreezing agent into a sanding container;
2) And then adding a dispersion medium into the sanding container, grinding for 1-5 hours, and filtering after grinding to obtain the product.
In some preferred embodiments, the controlled grinding speed of the grinding in the step 2) is 1500-2000r/min.
The third aspect of the invention provides an application of a fluopicolide-dimethomorph composition in the control of crop downy mildew.
Further preferably, the fluopicolide-dimethomorph composition is applied to control of cucumber downy mildew.
Has the advantages that: compared with the prior art, the fluopicolide-dimethomorph composition prepared by the invention has the following advantages:
1. the fluopicolide-dimethomorph composition prepared by the invention has better control effect on cucumber downy mildew, and the weight ratio of the fluopicolide to the dimethomorph is controlled to be 1:3, the control efficiency reaches 80.3 to 84.5 percent after 7 days, the disease index is controlled to be below 4.7, the harm of cucumber downy mildew is reduced, and the control effect is better;
2. the fluopicolide-dimethomorph composition provided by the invention has better effect on crops planted in soil in which other crops are sown within one year in the using process;
3. the fluopicolide-dimethomorph composition provided by the invention is prepared from ethylene oxide propylene oxide copolymer, acrylic acid crotonic acid copolymer and polyoxyethylene ether ammonium sulfate salt in a weight ratio of (1-5): (1-3): 1, the compatibility of substances among the compositions is greatly improved; when the suspending agent is prepared, the heat storage stability of the suspending agent can be ensured, the stability of the suspending agent in the storage process is improved, and the requirement of long-term storage is met;
4. the fluopicolide-dimethomorph composition provided by the invention can control the shear viscosity of a system to be 200-400mPa & s on the premise of improving the activity of fluopicolide and dimethomorph, and ensures that the suspension stability of the composition reaches more than 99%.
Drawings
FIG. 1 is a table of average disease indexes for controlling cucumber downy mildew in examples 1-4 of the present application;
FIG. 2 is a pre-drug grading disease index table for controlling cucumber downy mildew in examples 1-4 of the present application;
FIG. 3 is a table of disease grading for 7 days after 2 applications of examples 1-4 of the present application for controlling cucumber downy mildew.
Detailed Description
Examples
Example 1
A fluopicolide-dimethomorph composition is prepared from the following raw materials in percentage by weight: 10% of fluopicolide, 30% of dimethomorph, 3% of alkane oxygen-containing derivative copolymer, 2% of carboxylic acid-containing copolymer, 1% of ammonium sulfate salt, 0.5% of magnesium aluminum silicate, 0.5% of white carbon black, 4% of antifreezing agent, 0.3% of preservative, 0.15% of thickening agent, 0.1% of pH regulator, 0.3% of defoaming agent and the balance of dispersion medium to 100%.
The alkane oxygen-containing derivative copolymer is an ethylene oxide propylene oxide copolymer;
the carboxylic acid-containing copolymer is acrylic acid butenoic acid copolymer;
the ammonium sulfate salt is polyoxyethylene ether ammonium sulfate salt;
ethylene oxide propylene oxide copolymer available from Jiangsu Optimus chemical technology Limited; acrylic acid crotonic acid copolymer, available from Jiangsu Optimus chemical technology Limited; polyoxyethylene ether ammonium sulfate, commercially available from Nanjing Taihua chemical Co., ltd.
The particle size of the aluminum-magnesium silicate is 1000nm, and the aluminum-magnesium silicate is purchased from New Dilute metallurgy chemical Co., ltd, guangzhou city;
the antifreezing agent is ethylene glycol;
the preservative is sodium benzoate;
the thickening agent is xanthan gum;
the pH regulator is citric acid;
the defoaming agent is a polysiloxane defoaming agent, the viscosity of the defoaming agent is 160-200mPa & s (20 ℃), and the defoaming agent is purchased from a Heian petrochemical plant in Jiangsu province.
The dispersion medium is water.
A preparation method of a fluopicolide-dimethomorph composition comprises the following steps:
1) Adding fluopicolide, dimethomorph, alkane oxygen-containing derivative copolymer, carboxylic acid-containing copolymer, ammonium sulfate salt, magnesium aluminum silicate, a thickening agent, a defoaming agent and an antifreezing agent into a sanding container;
2) And then adding a dispersion medium into the sanding container, grinding at the grinding speed of 1800r/min for 2 hours, and filtering after grinding to obtain the product.
Example 2
A fluopicolide composition comprises the following preparation raw materials in percentage by weight: 40% of fluopicolide, 3% of alkane oxygen-containing derivative copolymer, 2% of carboxylic acid-containing copolymer, 1% of ammonium sulfate, 0.5% of magnesium aluminum silicate, 0.5% of white carbon black, 4% of antifreezing agent, 0.3% of preservative, 0.15% of thickening agent, 0.1% of pH regulator, 0.3% of defoaming agent and the balance of dispersion medium to 100%.
The alkane oxygen-containing derivative copolymer is an ethylene oxide propylene oxide copolymer;
the carboxylic acid-containing copolymer is acrylic acid butenoic acid copolymer;
the ammonium sulfate salt is polyoxyethylene ether ammonium sulfate salt;
ethylene oxide propylene oxide copolymer available from Jiangsu Optimus chemical technology Limited; acrylic acid butenoic acid copolymer, available from Jiangsu Qingyu chemical technology Co., ltd; polyoxyethylene Ether ammonium sulfate, commercially available from Nanjing Taihua chemical Co., ltd.
The particle size of the magnesium aluminum silicate is 1000nm, and the magnesium aluminum silicate is purchased from Xinxiu metallurgy chemical industry Co., ltd;
the antifreezing agent is ethylene glycol;
the preservative is sodium benzoate;
the thickening agent is xanthan gum;
the pH regulator is citric acid;
the defoaming agent is polysiloxane defoaming agent with the viscosity of 160-200mPa s (20 ℃), and is purchased from Haian petrochemical plants in Jiangsu province.
The dispersion medium is water.
A preparation method of a fluopicolide-dimethomorph composition comprises the following steps:
1) Adding fluopicolide, alkane oxygenated derivative copolymer, carboxylic acid-containing copolymer, ammonium sulfate salt, magnesium aluminum silicate, thickening agent, defoaming agent and antifreezing agent into a sanding container;
2) And then adding a dispersion medium into the sanding container, grinding at the grinding speed of 1800r/min for 2 hours, and filtering after grinding to obtain the product.
Example 3
The dimethomorph-containing composition comprises the following preparation raw materials in percentage by weight: 40% of dimethomorph, 3% of alkane oxygen-containing derivative copolymer, 2% of carboxylic acid-containing copolymer, 1% of ammonium sulfate salt, 0.5% of magnesium aluminum silicate, 0.5% of white carbon black, 4% of antifreezing agent, 0.3% of preservative, 0.15% of thickening agent, 0.1% of pH regulator, 0.3% of defoaming agent and the balance of dispersion medium to 100%.
The alkane oxygen-containing derivative copolymer is an ethylene oxide-propylene oxide copolymer;
the carboxylic acid copolymer is acrylic butenoic acid copolymer;
the ammonium sulfate salt is polyoxyethylene ether ammonium sulfate salt;
ethylene oxide propylene oxide copolymer available from Jiangsu Optimus chemical technology Limited; acrylic acid crotonic acid copolymer, available from Jiangsu Optimus chemical technology Limited; polyoxyethylene Ether ammonium sulfate, commercially available from Nanjing Taihua chemical Co., ltd.
The particle size of the magnesium aluminum silicate is 1000nm, and the magnesium aluminum silicate is purchased from Xinxiu metallurgy chemical industry Co., ltd;
the antifreezing agent is ethylene glycol;
the preservative is sodium benzoate;
the thickening agent is xanthan gum;
the pH regulator is citric acid;
the defoaming agent is a polysiloxane defoaming agent, the viscosity of the defoaming agent is 160-200mPa & s (20 ℃), and the defoaming agent is purchased from a Heian petrochemical plant in Jiangsu province.
The dispersion medium is water.
A preparation method of a fluopicolide-dimethomorph composition comprises the following steps:
1) Adding dimethomorph, alkane oxygen-containing derivative copolymer, carboxylic acid-containing copolymer, ammonium sulfate salt, magnesium aluminum silicate, thickening agent, defoaming agent and antifreezing agent into a sanding container;
2) And then adding a dispersion medium into the sanding container, grinding at the grinding speed of 1800r/min for 2 hours, and filtering after grinding to obtain the product.
Example 4
A fluopicolide-dimethomorph composition is prepared from the following raw materials in percentage by weight: 10% of fluopicolide, 30% of dimethomorph and the balance of dispersion medium to 100%.
The dispersion medium is water.
A preparation method of a fluopicolide-dimethomorph composition comprises the following steps:
1) Adding fluopicolide and dimethomorph into a sanding container;
2) And then adding a dispersion medium into the sanding container, grinding at the grinding speed of 1800r/min for 2 hours, and filtering after grinding to obtain the product.
Example 5
A fluopicolide-dimethomorph composition is prepared from the following raw materials in percentage by weight: 10% of fluopicolide, 30% of dimethomorph, 3% of alkane oxygen-containing derivative copolymer, 1% of ammonium sulfate, 0.5% of magnesium aluminum silicate, 0.5% of white carbon black, 4% of an antifreezing agent, 0.3% of a preservative, 0.15% of a thickening agent, 0.1% of a pH regulator, 0.3% of an antifoaming agent, and the balance of a dispersion medium to 100%.
The alkane oxygen-containing derivative copolymer is an ethylene oxide propylene oxide copolymer;
the ammonium sulfate salt is polyoxyethylene ether ammonium sulfate salt;
ethylene oxide propylene oxide copolymer available from Jiangsu Optimus chemical technology Limited; acrylic acid butenoic acid copolymer, available from Jiangsu Qingyu chemical technology Co., ltd; polyoxyethylene ether ammonium sulfate, commercially available from Nanjing Taihua chemical Co., ltd.
The particle size of the aluminum-magnesium silicate is 1000nm, and the aluminum-magnesium silicate is purchased from New Dilute metallurgy chemical Co., ltd, guangzhou city;
the antifreezing agent is ethylene glycol;
the preservative is sodium benzoate;
the thickening agent is xanthan gum;
the pH regulator is citric acid;
the defoaming agent is a polysiloxane defoaming agent, the viscosity of the defoaming agent is 160-200mPa & s (20 ℃), and the defoaming agent is purchased from a Heian petrochemical plant in Jiangsu province.
The dispersion medium is water.
A preparation method of a fluopicolide-dimethomorph composition comprises the following steps:
1) Adding fluopicolide, dimethomorph, alkane oxygenated derivative copolymer, ammonium sulfate salt, magnesium aluminum silicate, a thickening agent, a defoaming agent and an antifreezing agent into a sanding container;
2) And then adding a dispersion medium into the sanding container, grinding at the grinding speed of 1800r/min for 2 hours, and filtering after grinding to obtain the product.
Example 6
A fluopicolide-dimethomorph composition is prepared from the following raw materials in percentage by weight: 10% of fluopicolide, 30% of dimethomorph, 3% of alkane oxygen-containing derivative copolymer, 2% of carboxylic acid-containing copolymer, 1% of ammonium sulfate salt, 0.5% of magnesium aluminum silicate, 0.5% of white carbon black, 4% of antifreezing agent, 0.3% of preservative, 0.15% of thickening agent, 0.1% of pH regulator, 0.3% of defoaming agent and the balance of dispersion medium to 100%.
The alkane oxygen-containing derivative copolymer is an ethylene oxide propylene oxide copolymer;
the carboxylic acid-containing copolymer is acrylic acid butenoic acid copolymer;
the ammonium sulfate salt is polyoxyethylene ether ammonium sulfate salt;
ethylene oxide propylene oxide copolymer available from Jiangsu Optimus chemical technology Limited; acrylic acid crotonic acid copolymer, available from Jiangsu Optimus chemical technology Limited; polyoxyethylene ether ammonium sulfate, commercially available from Nanjing Taihua chemical Co., ltd.
The particle size of the aluminum-magnesium silicate is 2000nm, and the aluminum-magnesium silicate is purchased from New Dilute metallurgy chemical Co., ltd of Guangzhou city;
the antifreezing agent is ethylene glycol;
the preservative is sodium benzoate;
the thickening agent is xanthan gum;
the pH regulator is citric acid;
the defoaming agent is a polysiloxane defoaming agent, the viscosity of the defoaming agent is 160-200mPa & s (20 ℃), and the defoaming agent is purchased from a Heian petrochemical plant in Jiangsu province.
The dispersion medium is water.
A preparation method of a fluopicolide-dimethomorph composition comprises the following steps:
1) Adding fluopicolide, dimethomorph, alkane oxygen-containing derivative copolymer, carboxylic acid-containing copolymer, ammonium sulfate salt, magnesium aluminum silicate, a thickening agent, a defoaming agent and an antifreezing agent into a sanding container;
2) And then adding a dispersion medium into the sanding container, grinding at the grinding speed of 1800r/min for 2 hours, and filtering after grinding to obtain the product.
And (3) performance testing:
1. and (3) field experiments:
when the fluopicolide/dimethomorph composition prepared in example 1 was subjected to an experiment, the composition was divided into three cases, namely, experiments using 15 ml, 30ml and 45 ml per mu of land, which are respectively designated as SA, SB and SC.
The fluopicolide/dimethomorph compositions (SA, SB, SC) prepared in example 1 and example 2 (SD, 50 ml/acre of formulation amount per acre of land), example 3 (SE, 17 ml/acre of formulation amount per acre of land), example 4 (SF, 30 ml/acre of formulation amount per acre of land), and the clear water control group (G) were subjected to a control effect test as follows:
1. cell arrangement
SD1 SA2 SE3 SF4
SB1 SF2 SC3 SD4
SF1 SC2 G3 SA4
SE1 SB2 SF3 G4
SC1 G2 SD3 SE4
SA1 SE2 SB3 SC4
G1 SD2 SA3 SB4
2. Cell area and repetition
Cell area 20m 2 4 repeats;
3. method of administering a drug
Time period 3.1 and method
Crop: cucumber, variety: jinyou No. 1, the second dilution method is adopted to prepare the liquid medicine at the flowering and fruiting period of cucumber and the initial stage of downy mildew when the No. 1 pesticide is applied, and the liquid medicine is uniformly sprayed by a sprayer.
3.2 applicator devices
Spraying with a sprayer of model HD400 of agricultural industry, wherein the spraying pressure is 0.2-0.4MPa, the diameter of a spray hole is 1mm, the flow rate is 730ml/min, and the corrected error is within 10%.
3.3 times
The application is carried out for 2 times.
3.4 capacity of use
The water consumption per community is about 1.25-1.5 liters, and the water consumption per hectare is about 625-750 liters.
4. Investigation method
Sampling was performed at 4 random points per cell, 2 plants were investigated at each point, and all leaves were investigated at each plant. The total leaf number and the diseased leaf number at each level were recorded as follows:
level 0: no disease spots;
level 1: the lesion area accounts for less than 5% of the whole leaf area;
and 3, level: the lesion area accounts for 6 to 10 percent of the whole leaf area;
and 5, stage: the lesion area accounts for 11% -25% of the whole leaf area;
and 7, stage: the lesion area accounts for 26-50% of the whole leaf area;
and 9, stage: the lesion area accounts for more than 50% of the whole leaf area.
5. Drug effect calculation method
Figure BDA0003262385610000121
Figure BDA0003262385610000122
Wherein PT 0 : pre-drug condition in drug treatment areaAn index;
PT 1 : post-drug disease index in the drug treatment area;
CK 0 : clear water control area pre-drug disease index;
CK 1 : clear water controls the post-drug disease index in the area.
6. The weather conditions at the test sites during the test are tabulated as follows:
Figure BDA0003262385610000123
Figure BDA0003262385610000131
the results of the experiment are reported in the following table:
Figure BDA0003262385610000132
where the data in the table are averages of 4 replicates and the letters indicate significance of difference (upper case 0.01 level, lower case 0.05 level).
15 ml, 30ml and 45 ml of fluopicolide-dimethomorph composition prepared in the example 1 are used for controlling cucumber downy mildew, the control effect is respectively 62.8%, 80.3% and 84.5% 7 days after 2 times of application, and the control effect is respectively 56.5%, 78.5% and 82.3% 14 days after 2 times of application. The fluopicolide-dimethomorph composition prepared in the example 2 is used for 50 milliliters of land, and the control effect is 71.7 percent and 68.4 percent respectively after 7 days and 14 days after 2 times of application. The product prepared in example 3 is used for 17 ml per mu, and the control effect is respectively 74.4% and 74.9% 7 and 14 days after 2 times of application. The product prepared in the example 4 is used for 30 milliliters per mu, and the control effect is 78.9 percent and 78 percent respectively after 7 and 14 days after 2 times of application. The control statistical data of 7 days after 2 times of application is used for variance analysis, the control effect of 30 milliliters and 45 milliliters of test agents for each mu is equivalent to and obviously higher than 15 milliliters of the control effect for each mu, and compared with examples 2, 3 and 4, the control effect of 30 milliliters and 45 milliliters of the composition prepared in the example 1 for each mu is equivalent to and obviously higher than the control effect of 30 milliliters of the product prepared in the example 4 for each mu and 50 milliliters of the product prepared in the example 2 for each mu; the control effect difference between 30ml of the composition prepared in example 1 and 17 ml of the product prepared in example 3 is not significant, and the control effect difference between 15 ml of the composition prepared in example 1 and 50 ml of the product prepared in example 2 is equivalent.
Test results show that the composition prepared in the example 1 can prevent and treat cucumber downy mildew, the prevention effect is improved along with the increase of the dosage, the dosage of 15 ml is lower for each mu, the prevention effect is 80.3-84.5% 7 days after 30 and 45 ml 2 times of medicine is taken for each mu, the disease index is controlled to be below 4.7 and is far lower than 23.2 of a clear water control disease index, the harm of the cucumber downy mildew is reduced, and the prevention effect is better; the control effect is still maintained to be more than 78.5 percent in 14 days after 2 times of medicine application, and the good persistence is shown. During the test period, the cucumber grows normally, and no phytotoxicity symptom is observed. The composition prepared in example 1 can be used for controlling cucumber downy mildew.
The average disease index for preventing and treating cucumber downy mildew of the composition, the grading disease index before the composition is used for preventing and treating cucumber downy mildew, and the grading disease index 7 days after the composition is used for preventing and treating cucumber downy mildew 2 times are shown in figures 1, 2 and 3.
2. Stability test
1. Heat storage stability test: the combinations prepared in example 1 and examples 5 and 6 were used for the heat storage stability tests and the test results are reported in the table below.
The test method comprises the following steps: the prepared sample was sealed in a 10 ml ampoule, left at 54 ℃ for two weeks, and observed for changes in surface, and if there was no change, the heat storage was regarded as passed, otherwise, it was regarded as failed.
2. And (3) suspension stability test: the combinations prepared in example 1 and examples 5, 6 were used for suspension stability testing and the results are reported in the table below.
Test methods reference: GB/T14825-2006.
Experiment of Stability to Heat storage Suspension rate/%
Example 1 Qualified 99.2
Example 5 Fail to be qualified 89.5
Example 6 Fail to be qualified 88.4

Claims (10)

1. A fluopicolide-dimethomorph composition is characterized by comprising the following raw materials: fluopicolide and dimethomorph; the weight ratio of fluopicolide to dimethomorph is 1: (1-5).
2. The fluopicolide-dimethomorph composition according to claim 1, wherein the weight ratio of fluopicolide to dimethomorph is 1: (2-4).
3. The fluopicolide-dimethomorph composition according to claim 1 or 2, wherein the preparation raw material further comprises at least one of an alkane oxy-derivative copolymer, a carboxylic acid-containing copolymer, a sulfate, an ammonium sulfate salt and a sulfonate.
4. The fluopicolide-dimethomorph composition according to claim 3, wherein the starting materials for the preparation further comprise an alkane oxy-derivative copolymer, a carboxylic acid-containing copolymer and an ammonium sulfate salt.
5. A fluopicolide-dimethomorph composition according to claim 4, wherein the weight ratio of the alkane oxygen-containing derivative copolymer, the carboxylic acid-containing copolymer and the ammonium sulfate salt is (1-5): (1-3): 1.
6. the fluopicolide-dimethomorph composition according to claim 4, wherein the raw materials for preparation further comprise magnesium aluminum silicate, and the particle size of the magnesium aluminum silicate is 300-5000nm.
7. The fluopicolide-dimethomorph composition according to claim 6, wherein the raw materials for preparation further comprise a thickener, an antifoaming agent, a dispersion medium and an antifreezing agent.
8. A process for the preparation of a fluopicolide-dimethomorph composition according to claim 7, comprising the steps of:
1) Adding fluopicolide, dimethomorph, alkane oxygen-containing derivative copolymer, carboxylic acid-containing copolymer, ammonium sulfate salt, magnesium aluminum silicate, a thickening agent, a defoaming agent and an antifreezing agent into a sanding container;
2) And then adding a dispersion medium into the sanding container, grinding for 1-5 hours, and filtering after grinding to obtain the product.
9. The method for preparing fluopicolide-dimethomorph composition according to claim 8, wherein the controlled polishing rate in the step 2) is 1500 to 2000r/min.
10. Use of a fluopicolide-dimethomorph composition according to any one of claims 1 to 8 for the control of crop downy mildew.
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