CN112806379B - Hexaconazole-kresoxim-methyl suspending agent and preparation method thereof - Google Patents
Hexaconazole-kresoxim-methyl suspending agent and preparation method thereof Download PDFInfo
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- CN112806379B CN112806379B CN202011619756.6A CN202011619756A CN112806379B CN 112806379 B CN112806379 B CN 112806379B CN 202011619756 A CN202011619756 A CN 202011619756A CN 112806379 B CN112806379 B CN 112806379B
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION 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
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/64—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with three nitrogen atoms as the only ring hetero atoms
- A01N43/647—Triazoles; Hydrogenated triazoles
- A01N43/653—1,2,4-Triazoles; Hydrogenated 1,2,4-triazoles
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION 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
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/02—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing liquids as carriers, diluents or solvents
- A01N25/04—Dispersions, emulsions, suspoemulsions, suspension concentrates or gels
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION 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
- A01N37/00—Biocides, 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
- A01N37/44—Biocides, 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 nitrogen atom attached to the same carbon skeleton by a single or double bond, this nitrogen atom not being a member of a derivative or of a thio analogue of a carboxylic group, e.g. amino-carboxylic acids
- A01N37/50—Biocides, 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 nitrogen atom attached to the same carbon skeleton by a single or double bond, this nitrogen atom not being a member of a derivative or of a thio analogue of a carboxylic group, e.g. amino-carboxylic acids the nitrogen atom being doubly bound to the carbon skeleton
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- Plant Pathology (AREA)
- Engineering & Computer Science (AREA)
- Pest Control & Pesticides (AREA)
- Agronomy & Crop Science (AREA)
- Wood Science & Technology (AREA)
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Abstract
The application relates to the field of agricultural bactericides and particularly discloses a hexaconazole-kresoxim-methyl suspending agent and a preparation method thereof. The hexaconazole-kresoxim-methyl suspending agent comprises the following components in parts by weight, a hexaconazole raw drug, a kresoxim-methyl raw drug, a thickening agent, a dispersing agent, an adhesive, a preservative, an antifoaming agent and purified water, wherein the preservative comprises sodium benzoate and carbazone, and the adhesive comprises ammonium formate and xanthan gum; the preparation method comprises the steps of taking part of purified water, adding hexaconazole original drug, kresoxim-methyl original drug, thickening agent, dispersing agent, sodium benzoate and ammonium formate into the part of purified water, stirring, sanding to reach a qualified particle size, dissolving the carbazone and the xanthan gum by using the rest of purified water, mixing the two parts of mixed solution, and uniformly dispersing to obtain the suspending agent. The hexaconazole-kresoxim-methyl suspending agent can be used for preventing and treating apple powdery mildew, and has the advantages of reducing bactericide waste and improving prevention and treatment effects; in addition, the preparation method has the advantages of simple preparation and improvement of the control effect of the bactericide.
Description
Technical Field
The application relates to the field of agricultural bactericides, in particular to a hexaconazole-kresoxim-methyl suspending agent and a preparation method thereof.
Background
Agricultural fungicides are a class of pesticides used to control plant diseases caused by various pathogenic microorganisms, generally referred to as fungicides. But internationally, it is generally a generic term for agents for controlling various types of pathogenic microorganisms. Along with the development of bactericides, virucides, algicides and other subclasses are distinguished.
In the related art, the chinese patent application with publication number CN101999364A discloses a bactericidal composition containing hexaconazole, the active ingredients of which contain hexaconazole and kresoxim-methyl; when the composition is prepared into a suspending agent, the suspending agent comprises the following components, by weight, 1-50% of hexaconazole, 1-50% of kresoxim-methyl, 2-10% of dispersing agent, 2-10% of wetting agent, 0.1-1% of defoaming agent, 0.1-2% of thickening agent, 0.1-8% of antifreeze agent and 100% of deionized water; the dispersing agent, the wetting agent, the defoaming agent, the thickening agent and the antifreezing agent in the formula are sheared and mixed uniformly at a high speed, hexaconazole and kresoxim-methyl are added, and ball milling is carried out in a ball mill for 2-3 hours to ensure that the particle size of particles is below 5 mu m, so as to prepare the hexaconazole-kresoxim-methyl suspending agent product.
Aiming at the related technologies, the inventor thinks that the prepared hexaconazole-kresoxim-methyl suspending agent is sprayed on the leaves, and dew drives the suspending agent on the surfaces of the leaves to slide down to soil after the dew is generated at night, thereby causing the waste of the suspending agent and reducing the control effect of the suspending agent.
Disclosure of Invention
In order to reduce the waste of the suspending agent and improve the control effect of the suspending agent, the application provides the hexaconazole-kresoxim-methyl suspending agent and the preparation method thereof.
In a first aspect, the application provides a hexaconazole-kresoxim-methyl suspending agent, which adopts the following technical scheme:
the hexaconazole-kresoxim-methyl suspending agent comprises, by weight, 16-28 parts of hexaconazole raw drug, 41-65 parts of kresoxim-methyl raw drug, 3-7 parts of thickening agent, 8-12 parts of dispersing agent, 6.2-14.6 parts of adhesive, 1.4-3.8 parts of preservative, 0.01-0.03 part of defoaming agent and 90-110 parts of purified water, wherein the preservative comprises sodium benzoate and cason, and the adhesive comprises ammonium formate and xanthan gum.
By adopting the technical scheme, because the ammonium formate and the xanthan gum are adopted as the adhesive, the adhesive strength of the hexaconazole raw drug and the kresoxim-methyl raw drug on the blades is increased through the synergistic effect of the ammonium formate and the xanthan gum, the waste of the hexaconazole raw drug and the kresoxim-methyl raw drug is reduced, and the control effect is effectively improved.
Preferably, the thickener comprises magnesium aluminum silicate and white carbon black, and the weight ratio of the magnesium aluminum silicate to the white carbon black is 1-3: 2-4.
By adopting the technical scheme, the viscosity of the suspending agent is improved by the magnesium aluminum silicate and the white carbon black, so that the hexaconazole raw drug and the kresoxim-methyl raw drug are uniformly dispersed by the dispersing agent, the suspension rate of the hexaconazole raw drug and the kresoxim-methyl raw drug in the suspending agent is improved, and the drug effect of the suspending agent is improved.
Preferably, the dispersing agent is SP-SC3266, and the weight ratio of the magnesium aluminum silicate to the white carbon black to the ammonium formate to the SP-SC3266 is 1-3: 2-4: 6-14: 8-12.
By adopting the technical scheme, after the viscosity of the suspending agent is improved by the magnesium aluminum silicate and the white carbon black, the ammonium formate is uniformly dispersed in the suspending agent by the SP-SC3266, so that the adhesion performance of the suspending agent is improved, and the control effect is improved.
Preferably, the weight ratio of the ammonium formate to the sodium benzoate to the kasong is 6-14: 1-3: 0.4-0.8.
By adopting the technical scheme, ammonium formate is weakly acidic after being dissolved in purified water, so that the performances of sodium benzoate and carbazone are enhanced, and the corrosion resistance of the suspending agent is further improved.
Preferably, the weight ratio of the ammonium formate to the xanthan gum is 6-14: 0.2-0.6.
By adopting the technical scheme, the ratio of the weight parts of the ammonium formate to the weight parts of the xanthan gum is limited, so that the performance of the adhesive is further improved, and the prevention and control effect is improved.
Preferably, the weight part ratio of the hexaconazole technical drug to the kresoxim-methyl technical drug to the ammonium formate is 20-24: 49-57: 9 to 11.
By adopting the technical scheme, the ammonium formate promotes hexaconazole and kresoxim-methyl to enter the leaves, so that the control effect is improved.
In a second aspect, the application provides a preparation method of hexaconazole-kresoxim-methyl suspending agent, which adopts the following technical scheme:
s1, preparing a first mixed solution:
weighing purified water accounting for 95% of the total weight of the purified water as a first solvent, adding hexaconazole, kresoxim-methyl, a thickening agent, a dispersing agent, ammonium formate and sodium benzoate into the first solvent while stirring, wherein the stirring speed is 1500r/min, stirring for 30min at the same rotating speed after the adding is finished, sanding for 3-5 times after the stirring is finished, and adding a defoaming agent after the sanding is finished to prepare a first mixed solution;
s2, preparing a second mixed solution:
taking the residual purified water accounting for 5 percent of the total weight of the purified water as a second solvent, adding the carbazone and the xanthan gum into the second solvent, and stirring at a stirring speed of 300r/min until the carbazone and the xanthan gum are completely and uniformly dissolved to prepare a second mixed solution;
s3, mixing and blending:
and mixing the first mixed solution and the second mixed solution, and dispersing for 30min at the rotating speed of 1500r/min to obtain a final product.
By adopting the technical scheme, the hexaconazole technical product, the kresoxim-methyl technical product, the thickening agent, the dispersing agent, the ammonium formate and the sodium benzoate are subjected to sanding to control the particle size, and then the easily soluble cason and the xanthan gum are dissolved and mixed to prepare the final product, so that the production process is simple and the operation is easy.
Preferably, the first mixed solution in S1 is sanded 3 times.
By adopting the technical scheme, the particle size of the thickening agent is limited, and the suspension percentage of the suspending agent is improved, so that the performance of the suspending agent is improved.
In summary, the present application has the following beneficial effects:
1. because this application adopts xanthan gum and ammonium formate as the adhesive to increase hexaconazole original medicine and the original medicine of kresoxim-methyl adhesion strength on the blade, reduce the suspending agent that slides down from the blade, owing to reduced the waste of suspending agent, improved prevention and cure effect.
2. In the application, hexaconazole raw drug and kresoxim-methyl raw drug are preferably adopted as sterilization components and enter the leaves through systemic absorption in plants, so that the hexaconazole raw drug and the kresoxim-methyl raw drug are absorbed into fungi by the fungi, and the effect of effectively killing the fungi is obtained.
4. The method of this application, the raw materials of powder class are carried out the sanding earlier through the sanding and are dissolved to increase the solubility of sodium benzoate, ammonium formate in purified water, thereby make sodium benzoate and ammonium formate disperse more evenly in the suspending agent, effectively strengthen the drug effect.
Detailed Description
Hexaconazole technical material was purchased from Shandong Zollingao Biotech limited; kresoxim-methyl raw pesticide is purchased from Shaanxi Kanze chemical technology Co., Ltd; the magnesium aluminum silicate is purchased from a spiritual life gold source mining processing factory; the white carbon black is purchased from Shijiazhuanjin and Nanochemical Co Ltd; ammonium formate is purchased from Shandong province, Jiahao Ye Biotech limited; xanthan gum is purchased from Shandong Doufeng chemical Co., Ltd; sodium benzoate was purchased from Shandong Nuanju Biotech Co., Ltd; kathon was purchased from Jinan bamboo chemical Co., Ltd; the defoaming agent is an organic silicon defoaming agent and is purchased from Nicoti Henxin chemical technology Co., Ltd; SP-SC3266 was purchased from Ongsu science and technology, Inc.
The present application will be described in further detail with reference to examples.
Examples
Example 1
S1, preparing a first mixed solution:
weighing 85.5kg of purified water as a first solvent, adding 16kg of hexaconazole original drug, 41kg of kresoxim-methyl original drug, 1kg of magnesium aluminum silicate, 2kg of white carbon black, 8kg of SP-SC3266, 6kg of ammonium formate and 1kg of sodium benzoate into the first solvent while stirring, wherein the stirring speed is 1500r/min, stirring for 30min at the same rotating speed after the addition is finished, sanding for 3 times after the stirring is finished, and adding a defoaming agent after the sanding is finished to prepare a first mixed solution;
s2, preparing a second mixed solution:
weighing 4.5kg of purified water as a second solvent, adding 0.4kg of kasong and 0.2kg of xanthan gum into the second solvent, and stirring at a stirring speed of 300r/min until the kasong and the xanthan gum are completely and uniformly dissolved to prepare a second mixed solution;
s3, mixing and blending:
and mixing the first mixed solution and the second mixed solution, and dispersing at the rotating speed of 1500r/min for 30min to obtain a final product.
Example 2
The difference from the example 1 is that 20kg of hexaconazole technical, 49kg of kresoxim-methyl technical and 9kg of ammonium formate are added into S1.
Example 3
The difference from example 2 is that 10kg of ammonium formate is added in S1.
Example 4
The difference from the example 3 is that 95kg of purified water, 22kg of hexaconazole technical product and 53kg of kresoxim-methyl technical product are added into S1. S2 was added 5kg of purified water, 0.6kg of cason and 0.4kg of xanthan gum.
Example 5
The difference from example 4 is that 10kg of SP-SC3266 was added to S1.
Example 6
The difference from example 5 is that the number of sand-milling in S1 was 4.
Example 7
The difference from example 6 is that 2kg of magnesium aluminum silicate, 3kg of white carbon black and 4kg of sodium benzoate are added to S1, and 0.02kg of defoaming agent is added after sanding.
Example 8
The difference from the example 7 is that 104.5kg of purified water, 24kg of hexaconazole technical, 57kg of kresoxim-methyl technical, 12kg of SP-SC3266, 11kg of ammonium formate and 3kg of sodium benzoate are added into S1, the sanding frequency is 5 times, and 0.03kg of defoaming agent is added after the sanding is finished. 5.5kg of purified water, 0.8kg of cason and 0.6kg of xanthan gum are added into S2.
Example 9
The difference from the example 8 is that 28kg of hexaconazole technical, 65kg of kresoxim-methyl technical and 14kg of ammonium formate are added into S1.
The formulation of examples 1-9 is shown in the following table,
TABLE 1 EXAMPLES 1 TO 9 COMPARATIVE TABLE
Comparative example
Comparative example 1
The difference from example 5 is that 10.4kg of ammonium formate was added in S1 and no xanthan gum was added in S2.
Comparative example 2
The difference from example 5 is that no ammonium formate was added in S1 and 10.4kg xanthan gum was added in S2.
Comparative example 3
The difference from the example 5 is that magnesium aluminum silicate and white carbon black are not added in S1.
Comparative example 4
The difference from example 5 is that the number of sand-milling in S1 was 1.
Comparative example 5
The difference from example 5 is that the number of sand-milling in S1 was 7.
The proportions of comparative examples 1 to 5 are shown in the following table,
TABLE 2 COMPARATIVE EXAMPLES 1-5 COMPARATIVE EXAMPLES
Performance test
The performance of the suspending agents prepared in the examples 1-9 and the comparative examples 1-5 is detected according to Q/370112SDH 010-2021 & lt 35% hexaconazole-kresoxim-methyl suspending agent & gt.
TABLE 2 Performance test tables for examples 1 to 9 and comparative examples 1 to 5
The suspending agent prepared by the application can be used for preventing and treating powdery mildew, and the prevention and treatment effect is detected according to GB/T17980.30-2000 'pesticide field efficacy test criterion (I) bactericide for preventing and treating cucumber powdery mildew'.
TABLE 4 Table of controlling effect of examples 1 to 9 and comparative examples 1 to 5
It can be seen by combining example 5 and comparative example 1 and combining tables 3 and 4 that the control effect is greatly reduced when the adhesive is only ammonium formate, probably because the adhesive strength of the suspending agent on the leaves is insufficient due to lack of xanthan gum thickening, the suspending agent slides off the leaves after being sprayed on the leaves, and the hexaconazole technical product and the kresoxim-methyl technical product entering the leaves of the suspending agent are reduced, thereby reducing the control effect.
As can be seen by combining example 5 and comparative example 2 and combining tables 3 and 4, when the adhesive agent is only xanthan gum, the control effect is greatly reduced, probably because the xanthan gum adheres hexaconazole technical drug and kresoxim-methyl technical drug as suspending agents and ammonium formate to the leaves after the suspending agents are sprayed on the leaves; after the water of the suspending agent is evaporated, the ammonium formate becomes solid and adheres to the blades, the suspending agent hexaconazole raw drug and the kresoxim-methyl raw drug adhere with the blades, when dew is generated at night, the ammonium formate absorbs moisture, so that the adhesion strength of the ammonium formate and the blades is increased, the hexaconazole raw drug and the kresoxim-methyl raw drug adhere to the blades, and the hexaconazole raw drug and the kresoxim-methyl raw drug are reduced from slipping along with the dew. After the dew is combined with the ammonium formate, the ammonium formate is partially dissolved and coated on the outer surfaces of the hexaconazole raw drug and the kresoxim-methyl raw drug and wraps the hexaconazole raw drug and the kresoxim-methyl raw drug into the leaves, so that the control effect is further improved.
As can be seen by combining example 5 and comparative example 2 with tables 3 and 4, in the absence of ammonium formate, sodium benzoate and cason are not in a weakly acidic environment, so that the corrosion preventing property is lowered, thereby lowering the heat storage stability and the low temperature stability.
By combining the example 5 and the comparative example 3 and combining the tables 3 and 4, it can be seen that the suspension rate of the suspending agent is increased by adding the thickening agent, the dispersion uniformity and the suspension stability of the hexaconazole technical material and the kresoxim-methyl technical material are improved, and the control effect is effectively improved.
As can be seen by combining example 5 and comparative example 4 and combining tables 3 and 4, insufficient sanding times leads to a large particle size of the thickener, resulting in insufficient suspension rates of hexaconazole and kresoxim-methyl in the suspension, and thus leading to a reduction in control effect.
It can be seen by combining example 5 and comparative example 5 and tables 3 and 4 that too many times of sanding lead to a smaller particle size of the thickener, thus enhancing the fluidity of the suspending agent, leading to insufficient adhesive strength of the suspending agent on the blades, and causing the hexaconazole technical and the kresoxim-methyl technical to easily slide off the blades, leading to a reduction in the control effect.
The present embodiment is only for explaining the present application, and it is not limited to the present application, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present application.
Claims (2)
1. The hexaconazole-kresoxim-methyl suspending agent is characterized by comprising the following components in parts by weight of 16-28 parts of hexaconazole raw drug, 41-65 parts of kresoxim-methyl raw drug, 3-7 parts of thickening agent, 8-12 parts of dispersing agent, 6.2-14.6 parts of adhesive and preservative: 1.4-3.8 parts of defoaming agent, 0.01-0.03 part of purified water and 90-110 parts of purified water, wherein the adhesive is composed of ammonium formate and xanthan gum; the weight ratio of the ammonium formate to the xanthan gum is 6-14: 0.2-0.6, the preservative is composed of sodium benzoate and kason, the weight ratio of the ammonium formate to the sodium benzoate to the kason is 6-14: 1-3: 0.4-0.8, the weight ratio of the hexaconazole original drug to the kresoxim-methyl original drug to the ammonium formate is 20-24: 49-57: 9-11, wherein the thickening agent consists of magnesium aluminum silicate and white carbon black, the weight ratio of the magnesium aluminum silicate to the white carbon black is 1-3: 2-4, and the dispersing agent is SP-SC 3266; s1, preparing a first mixed solution, namely weighing purified water accounting for 95% of the total weight of the purified water as a first solvent, adding hexaconazole, kresoxim-methyl, a thickening agent, a dispersing agent, ammonium formate and sodium benzoate into the first solvent while stirring, wherein the stirring speed is 1500r/min, stirring for 30min at the same rotating speed after the addition is finished, sanding for 3 times after the stirring is finished, and adding a defoaming agent after the sanding is finished to prepare the first mixed solution; s2, preparing a second mixed solution, namely, taking the purified water accounting for 5 percent of the total weight of the purified water as a second solvent, adding the kaempferia galanga and the xanthan gum into the second solvent, and stirring at a stirring speed of 300r/min until the kaempferia galanga and the xanthan gum are completely and uniformly dissolved to prepare the second mixed solution; and S3, mixing and blending, namely mixing the first mixed solution and the second mixed solution, and dispersing for 30min at the rotating speed of 1500r/min to obtain a final product.
2. The hexaconazole-kresoxim-methyl suspending agent as defined in claim 1, wherein the weight ratio of magnesium aluminum silicate, white carbon black, ammonium formate and SP-SC3266 is 1-3: 2-4: 6-14: 8-12.
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| CN101999364A (en) * | 2010-12-02 | 2011-04-06 | 陕西美邦农药有限公司 | Hexaconazole-containing germicide composition |
| FR2997605B1 (en) * | 2012-11-08 | 2015-12-11 | Rhodia Operations | AQUEOUS SUSPENSIONS FOR AGRICULTURAL COMPOSITIONS |
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