CN113582756A - Pesticide fertilizer containing metalaxyl-M and hymexazol for preventing and treating damping off and application thereof - Google Patents
Pesticide fertilizer containing metalaxyl-M and hymexazol for preventing and treating damping off and application thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05G—MIXTURES OF FERTILISERS COVERED INDIVIDUALLY BY DIFFERENT SUBCLASSES OF CLASS C05; MIXTURES OF ONE OR MORE FERTILISERS WITH MATERIALS NOT HAVING A SPECIFIC FERTILISING ACTIVITY, e.g. PESTICIDES, SOIL-CONDITIONERS, WETTING AGENTS; FERTILISERS CHARACTERISED BY THEIR FORM
- C05G3/00—Mixtures of one or more fertilisers with additives not having a specially fertilising activity
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01G—HORTICULTURE; CULTIVATION OF VEGETABLES, FLOWERS, RICE, FRUIT, VINES, HOPS OR SEAWEED; FORESTRY; WATERING
- A01G13/00—Protecting plants
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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
- A01N25/26—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 in coated particulate form
- A01N25/28—Microcapsules or nanocapsules
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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
- A01N37/46—N-acyl derivatives
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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
- A01N43/72—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with nitrogen atoms and oxygen or sulfur atoms as ring hetero atoms
- A01N43/80—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with nitrogen atoms and oxygen or sulfur atoms as ring hetero atoms five-membered rings with one nitrogen atom and either one oxygen atom or one sulfur atom in positions 1,2
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05B—PHOSPHATIC FERTILISERS
- C05B7/00—Fertilisers based essentially on alkali or ammonium orthophosphates
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05G—MIXTURES OF FERTILISERS COVERED INDIVIDUALLY BY DIFFERENT SUBCLASSES OF CLASS C05; MIXTURES OF ONE OR MORE FERTILISERS WITH MATERIALS NOT HAVING A SPECIFIC FERTILISING ACTIVITY, e.g. PESTICIDES, SOIL-CONDITIONERS, WETTING AGENTS; FERTILISERS CHARACTERISED BY THEIR FORM
- C05G3/00—Mixtures of one or more fertilisers with additives not having a specially fertilising activity
- C05G3/60—Biocides or preservatives, e.g. disinfectants, pesticides or herbicides; Pest repellants or attractants
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05G—MIXTURES OF FERTILISERS COVERED INDIVIDUALLY BY DIFFERENT SUBCLASSES OF CLASS C05; MIXTURES OF ONE OR MORE FERTILISERS WITH MATERIALS NOT HAVING A SPECIFIC FERTILISING ACTIVITY, e.g. PESTICIDES, SOIL-CONDITIONERS, WETTING AGENTS; FERTILISERS CHARACTERISED BY THEIR FORM
- C05G3/00—Mixtures of one or more fertilisers with additives not having a specially fertilising activity
- C05G3/80—Soil conditioners
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Abstract
The invention discloses a medicinal fertilizer containing metalaxyl-M and hymexazol for preventing and treating damping off and an application thereof, belonging to the technical field of medicinal fertilizers, and comprising the following raw materials in parts by mass: 15-20 parts of drug particles, 18-24 parts of potassium nitrate, 10-15 parts of diammonium phosphate and 18-22 parts of modified diatomite; the disintegrant added in the drug particles in the drug fertilizer takes lignocellulose as an initial raw material, has good structural viscosity and dispersibility, and the intermediate product 1 obtained after chloroacetic acid carboxymethylation has good water solubility; the rest hydroxyl of the intermediate product 1 is oxidized into aldehyde group after being treated by a sarrett reagent to obtain an intermediate product 2, the aldehyde group cannot be further oxidized into carboxyl, the intermediate product 2 and sorbitol further react to obtain a disintegrant, wherein the sorbitol has good water absorbability, and the disintegrant prepared by the method can absorb more water, is convenient for expansion and disintegration, increases the looseness of soil of a part where the pesticide and fertilizer are applied, and is beneficial to the growth of crops.
Description
Technical Field
The invention belongs to the technical field of pesticide fertilizers, and particularly relates to a pesticide fertilizer containing metalaxyl-M and hymexazol for preventing and treating damping off and an application thereof.
Background
metalaxyl-M is light brown and sticky transparent liquid, and has good control effect on diseases of vegetables, fruit trees, tobacco, oil plants, cotton, grains and other crops caused by downy mildew, phytophthora and pythium. The hymexazol is named as 3-hydroxy-5-methylisoxazole in chemical name, belongs to systemic efficient pesticide bactericide and soil disinfectant, is also a plant growth regulator, has the characteristics of high efficiency, low toxicity and no public nuisance, can effectively inhibit the normal growth of pathogenic fungi mycelium or directly kill germs, and can promote the growth of plants; and has the functions of promoting the growth and development of crop roots, rooting and strengthening seedlings and improving the survival rate of crops.
In agricultural production, pesticides and fertilizers are often applied at the same time so as to promote the healthy growth of crops, and in order to facilitate agricultural production, pesticide fertilizers prepared by mixing pesticides and fertilizers are available. The pesticide fertilizer is convenient to transport and store, and is generally prepared into granules or powder, and when in use, the pesticide fertilizer can be directly applied and watered, and can also be dissolved by water for reuse. However, metalaxyl-M is liquid at normal temperature, so that the metalaxyl-M is not convenient to prepare a solid medicinal fertilizer together with other raw materials, and if the metalaxyl-M is mixed into a solid material, the solid medicinal fertilizer is not convenient to disintegrate and is easy to harden.
Disclosure of Invention
The invention aims to provide a medicinal fertilizer containing metalaxyl-M and hymexazol for preventing and treating damping off and application thereof, so as to solve the problems in the background technology.
The purpose of the invention can be realized by the following technical scheme: the pesticide fertilizer containing metalaxyl-M and hymexazol for preventing and treating damping off comprises the following raw materials in parts by mass: 15-20 parts of drug particles, 18-24 parts of potassium nitrate, 10-15 parts of diammonium phosphate and 18-22 parts of modified diatomite;
the medicine granule comprises 5-8 parts of a component A, 8-10 parts of a component B and 3-5 parts of a disintegrating agent in parts by mass, and is prepared by the following steps:
the method comprises the following steps: adding metalaxyl-M into a flask, adding sodium dodecyl sulfate and distilled water with the volume of 10 times, and magnetically stirring for 15-20min under the condition of 6000-7200r/min to ensure that the liquid in the flask forms stable homogeneous emulsion; pretreating beta-cyclodextrin, mixing with the homogeneous emulsion, standing in a water bath for 3-3.5h, and performing aftertreatment to obtain a component A; wherein the temperature of the water bath is 50 ℃; the pretreatment step is to dissolve the beta-cyclodextrin by 7 times of volume and 70 ℃ of distilled water; the post-treatment step comprises washing the mixture after water bath with anhydrous ethanol for 2-3 times, infrared drying, and grinding into white powder.
Step two: adding hymexazol into a flask, adding distilled water, stirring, adding activator and carrageenan, stirring for 25-30min, adding modified resin, stirring, and infrared drying to obtain component B; the dosage ratio of hymexazol, activating agent, carrageenin and modified resin is 3 g: 0.8 g: 1.5 g: 8g of the total weight of the mixture; the activator is edetic acid and tartaric acid which are mixed according to the weight ratio of 7: 4; the modified resin is biodegradable resin purchased from Shanghai reduction polymer materials GmbH;
step three: mixing the component A, the component B and the disintegrating agent by a stirrer, wetting by absolute ethyl alcohol, and granulating by a granulator to obtain medicine granules.
The disintegrant is prepared by the following steps:
step S1: adding distilled water into a flask, adding lignocellulose, stirring for dissolving, heating to 55-60 ℃, slowly dropwise adding chloroacetic acid solution and sodium hydroxide solution into the solution, controlling the dropwise adding to be finished within 30-35min, carrying out heat preservation reaction for 2-3h, and carrying out post-treatment to obtain an intermediate product 1; the chloroacetic acid solution is a 20% aqueous solution in mass fraction, and the sodium hydroxide solution is a 15% aqueous solution in mass fraction; the post-treatment comprises cooling the reaction solution, performing column chromatography, washing with anhydrous ethanol for 2-3 times, and infrared drying; the dosage ratio of the lignocellulose to the distilled water to the chloroacetic acid to the sodium hydroxide solution is 5 g: 100mL of: 75mL is 100 mL;
the reaction process is as follows:
step S2: dissolving the intermediate product 1 with dichloromethane, adding acetic anhydride and silica gel, stirring for dissolving, adding a Sairett reagent, reacting for 45-50min, and performing post-treatment to obtain an intermediate product 2; the acetic anhydride can prevent atoms at beta-position of alcoholic hydroxyl group of the intermediate product 1 from being eliminated, and the silica gel can reduce the adsorption of chromate in the sarrett reagent on the intermediate product 1 and increase the yield of the product; the dosage ratio of the intermediate product 1, dichloromethane, acetic anhydride, silica gel and the sarrette reagent is 10 g: 500 mL: 20mL of: 15-20 g: 15 mL; the post-treatment step comprises filtering the reactant with silicon dioxide, washing the filtrate with ethyl acetate for 2-3 times, combining the organic phases, washing with saturated copper sulfate solution for 1-2 times, drying with anhydrous sodium sulfate and concentrating;
the reaction process is as follows:
step S3: adding sorbitol into a flask, adding an auxiliary agent, magnetically stirring for 20-30min, adding the intermediate product 2 and distilled water, stirring for reacting for 2.5-3.5h, and performing post-treatment to obtain a disintegrating agent; the dosage ratio of sorbitol, auxiliary agent, intermediate product 2 and distilled water is 0.05 mol: 30mL of: 0.1 mol: 60 mL; the auxiliary agent is concentrated sulfuric acid, phosphotungstic acid, methanol and dimethyl sulfoxide according to the dosage ratio of 8 mL: 0.02 mmol: 35mL of: 20mL of the extract is prepared; the post-treatment step comprises cooling the reaction solution, filtering, washing the filter cake with anhydrous ethanol for 3-5 times, and infrared drying;
the reaction process is as follows:
the preparation method of the pesticide fertilizer containing metalaxyl-M and hymexazol for preventing and treating damping off comprises the following steps:
and uniformly stirring the drug particles, the potassium nitrate, the diammonium phosphate and the modified diatomite by using a stirrer to obtain the drug fertilizer. The pesticide fertilizer containing metalaxyl-M and hymexazol for preventing and treating damping off can be applied to farmlands.
The invention has the beneficial effects that:
1. the medicinal components in the medicinal fertilizer are pretreated, wherein metalaxyl-M is liquid, and the liquid is complexed with beta-cyclodextrin to form microcapsules, so that the effective components are wrapped in the microcapsules, and the medicinal fertilizer is convenient to prepare for storage and use; the hymexazol has systemic property, and is compounded with the activator, the carrageenan and the modified resin to prepare the component B with the slow release function, so that the loss of effective ingredients due to the washing of irrigation water or rainwater is reduced, and the drug effect is ensured.
2. The disintegrant added in the drug particles in the drug fertilizer takes lignocellulose as an initial raw material, has good structural viscosity and dispersibility, and the intermediate product 1 obtained after chloroacetic acid carboxymethylation has good water solubility; the rest hydroxyl of the intermediate product 1 is oxidized into aldehyde group after being treated by a sarrett reagent to obtain an intermediate product 2, the aldehyde group cannot be further oxidized into carboxyl, the intermediate product 2 and sorbitol further react to obtain a disintegrant, wherein the sorbitol has good water absorbability, and the disintegrant prepared by the method can absorb more water, is convenient for expansion and disintegration, increases the looseness of soil of a part where the pesticide and fertilizer are applied, and is beneficial to the growth of crops.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The preparation of the disintegrating agent comprises the following steps:
step S1: adding distilled water into a flask, adding lignocellulose, stirring for dissolving, heating to 55 ℃, slowly dropwise adding chloroacetic acid solution and sodium hydroxide solution into the solution, controlling the dropwise adding to be finished within 30min, keeping the temperature for reaction for 2h, cooling the reaction solution, performing column chromatography, washing with absolute ethyl alcohol for 2 times, and performing infrared drying to obtain an intermediate product 1; the chloroacetic acid solution is a 20% aqueous solution in mass fraction, and the sodium hydroxide solution is a 15% aqueous solution in mass fraction; the dosage ratio of the lignocellulose to the distilled water to the chloroacetic acid to the sodium hydroxide solution is 5 g: 100mL of: 75mL is 100 mL;
step S2: dissolving the intermediate product 1 with dichloromethane, adding acetic anhydride and silica gel, stirring for dissolving, adding a sarrette reagent, reacting for 45min, filtering the reactant with silicon dioxide, washing the filtrate with ethyl acetate for 2 times, combining the organic phases, washing with a saturated copper sulfate solution for 1 time, drying with anhydrous sodium sulfate, and concentrating to obtain an intermediate product 2; the dosage ratio of the intermediate product 1, dichloromethane, acetic anhydride, silica gel and the sarrette reagent is 10 g: 500 mL: 20mL of: 15 g: 15 mL;
step S3: adding sorbitol into a flask, adding an auxiliary agent, magnetically stirring for 20min, adding the intermediate product 2 and distilled water, stirring for reaction for 2.5h, cooling the reaction liquid, performing suction filtration, washing a filter cake with absolute ethyl alcohol for 3 times, and performing infrared drying to obtain a disintegrant; the dosage ratio of sorbitol, auxiliary agent, intermediate product 2 and distilled water is 0.05 mol: 30mL of: 0.1 mol: 60 mL; the auxiliary agent is concentrated sulfuric acid, phosphotungstic acid, methanol and dimethyl sulfoxide according to the dosage ratio of 8 mL: 0.02 mmol: 35mL of: 20mL of the extract.
Example 2
The preparation of the disintegrating agent comprises the following steps:
step S1: adding distilled water into a flask, adding lignocellulose, stirring for dissolving, heating to 58 ℃, slowly dropwise adding chloroacetic acid solution and sodium hydroxide solution into the solution, controlling the dropwise adding to be finished within 32min, keeping the temperature for reaction for 2.5h, cooling the reaction solution, performing column chromatography, washing for 2 times by using absolute ethyl alcohol, and performing infrared drying to obtain an intermediate product 1; the chloroacetic acid solution is a 20% aqueous solution in mass fraction, and the sodium hydroxide solution is a 15% aqueous solution in mass fraction; the dosage ratio of the lignocellulose to the distilled water to the chloroacetic acid to the sodium hydroxide solution is 5 g: 100mL of: 75mL is 100 mL;
step S2: dissolving the intermediate product 1 with dichloromethane, adding acetic anhydride and silica gel, stirring for dissolving, adding a sarrette reagent, reacting for 48min, filtering the reactant with silicon dioxide, washing the filtrate with ethyl acetate for 2 times, combining the organic phases, washing with a saturated copper sulfate solution for 1 time, drying with anhydrous sodium sulfate, and concentrating to obtain an intermediate product 2; the dosage ratio of the intermediate product 1, dichloromethane, acetic anhydride, silica gel and the sarrette reagent is 10 g: 500 mL: 20mL of: 15 g: 15 mL;
step S3: adding sorbitol into a flask, adding an auxiliary agent, magnetically stirring for 25min, adding the intermediate product 2 and distilled water, stirring for reaction for 3h, cooling the reaction liquid, performing suction filtration, washing a filter cake with absolute ethyl alcohol for 4 times, and performing infrared drying to obtain a disintegrant; the dosage ratio of sorbitol, auxiliary agent, intermediate product 2 and distilled water is 0.05 mol: 30mL of: 0.1 mol: 60 mL; the auxiliary agent is concentrated sulfuric acid, phosphotungstic acid, methanol and dimethyl sulfoxide according to the dosage ratio of 8 mL: 0.02 mmol: 35mL of: 20mL of the extract.
Example 3
The preparation of the disintegrating agent comprises the following steps:
step S1: adding distilled water into a flask, adding lignocellulose, stirring for dissolving, heating to 60 ℃, slowly dropwise adding chloroacetic acid solution and sodium hydroxide solution into the solution, controlling the dropwise adding to be finished within 35min, keeping the temperature for reaction for 3h, cooling the reaction solution, performing column chromatography, washing with absolute ethyl alcohol for 2-3 times, and performing infrared drying to obtain an intermediate product 1; the chloroacetic acid solution is a 20% aqueous solution in mass fraction, and the sodium hydroxide solution is a 15% aqueous solution in mass fraction; the dosage ratio of the lignocellulose to the distilled water to the chloroacetic acid to the sodium hydroxide solution is 5 g: 100mL of: 75mL is 100 mL;
step S2: dissolving the intermediate product 1 with dichloromethane, adding acetic anhydride and silica gel, stirring for dissolving, adding a sarrette reagent, reacting for 50min, filtering the reactant with silicon dioxide, washing the filtrate with ethyl acetate for 2-3 times, combining the organic phases, washing with a saturated copper sulfate solution for 1-2 times, drying with anhydrous sodium sulfate, and concentrating to obtain an intermediate product 2; the dosage ratio of the intermediate product 1, dichloromethane, acetic anhydride, silica gel and the sarrette reagent is 10 g: 500 mL: 20mL of: 20 g: 15 mL;
step S3: adding sorbitol into a flask, adding an auxiliary agent, magnetically stirring for 30min, adding the intermediate product 2 and distilled water, stirring for reaction for 3.5h, cooling the reaction liquid, performing suction filtration, washing a filter cake with absolute ethyl alcohol for 5 times, and performing infrared drying to obtain a disintegrant; the dosage ratio of sorbitol, auxiliary agent, intermediate product 2 and distilled water is 0.05 mol: 30mL of: 0.1 mol: 60 mL; the auxiliary agent is concentrated sulfuric acid, phosphotungstic acid, methanol and dimethyl sulfoxide according to the dosage ratio of 8 mL: 0.02 mmol: 35mL of: 20mL of the extract.
Example 4
The preparation method comprises the following steps of preparing a medicine granule, wherein the medicine granule comprises a component A5 part, a component B8 part and a disintegrating agent 3 part by mass:
the method comprises the following steps: adding metalaxyl-M into a flask, adding sodium dodecyl sulfate and distilled water with the volume 10 times that of the flask, and magnetically stirring for 15min under the condition of 6000r/min to ensure that liquid in the flask forms stable homogeneous emulsion; dissolving beta-cyclodextrin with distilled water with volume of 7 times and temperature of 70 ℃, mixing with the homogeneous emulsion, standing in water bath for 3h, washing the mixture after water bath with absolute ethyl alcohol for 2 times, performing infrared drying, and grinding into white powder to obtain a component A; wherein the temperature of the water bath is 50 ℃;
step two: adding hymexazol into a flask, adding distilled water, stirring, adding activator and carrageenan, stirring for 25min, adding modified resin, stirring, and infrared drying to obtain component B; the dosage ratio of hymexazol, activating agent, carrageenin and modified resin is 3 g: 0.8 g: 1.5 g: 8g of the total weight of the mixture; the activator is edetic acid and tartaric acid which are mixed according to the weight ratio of 7: 4;
step three: the component a, the component B and the disintegrant obtained in example 3 were mixed with a stirrer, wetted with absolute ethanol, and granulated with a granulator to obtain drug granules.
Example 5
The preparation method comprises the following steps of preparing medicine granules, wherein the medicine granules comprise a component A6 part, a component B7 part and a disintegrating agent 4 part in parts by mass:
the method comprises the following steps: adding metalaxyl-M into a flask, adding sodium dodecyl sulfate and distilled water with the volume of 10 times, and magnetically stirring for 20min under the condition of 6700r/min to ensure that the liquid in the flask forms stable homogeneous emulsion; dissolving beta-cyclodextrin with distilled water with volume of 7 times and temperature of 70 ℃, mixing with the homogeneous emulsion, standing in water bath for 3h, washing the mixture after water bath with absolute ethyl alcohol for 2 times, performing infrared drying, and grinding into white powder to obtain a component A; wherein the temperature of the water bath is 50 ℃;
step two: adding hymexazol into a flask, adding distilled water, stirring, adding activator and carrageenan, stirring for 28min, adding modified resin, stirring, and infrared drying to obtain component B; the dosage ratio of hymexazol, activating agent, carrageenin and modified resin is 3 g: 0.8 g: 1.5 g: 8g of the total weight of the mixture; the activator is edetic acid and tartaric acid which are mixed according to the weight ratio of 7: 4;
step three: the component a, the component B and the disintegrant obtained in example 3 were mixed with a stirrer, wetted with absolute ethanol, and granulated with a granulator to obtain drug granules.
Example 6
The preparation method comprises the following steps of preparing medicine granules, wherein the medicine granules comprise 8 parts of a component A, 10 parts of a component B and 5 parts of a disintegrating agent in parts by mass:
the method comprises the following steps: adding metalaxyl-M into a flask, adding sodium dodecyl sulfate and distilled water with the volume 10 times of that of the flask, and magnetically stirring for 20min under the condition of 7200r/min to ensure that liquid in the flask forms stable homogeneous emulsion; dissolving beta-cyclodextrin with distilled water with volume of 7 times and temperature of 70 ℃, mixing with the homogeneous emulsion, standing in water bath for 3.5h, washing the mixture after water bath with absolute ethyl alcohol for 3 times, performing infrared drying, and grinding into white powder to obtain a component A; wherein the temperature of the water bath is 50 ℃;
step two: adding hymexazol into a flask, adding distilled water, stirring, adding activator and carrageenan, stirring for 30min, adding modified resin, stirring, and infrared drying to obtain component B; the dosage ratio of hymexazol, activating agent, carrageenin and modified resin is 3 g: 0.8 g: 1.5 g: 8g of the total weight of the mixture; the activator is edetic acid and tartaric acid which are mixed according to the weight ratio of 7: 4;
step three: the component a, the component B and the disintegrant obtained in example 3 were mixed with a stirrer, wetted with absolute ethanol, and granulated with a granulator to obtain drug granules.
Example 7
The method comprises the following steps of preparing a medicinal fertilizer containing metalaxyl-M and hymexazol for preventing and treating damping-off, wherein the medicinal fertilizer comprises 18 parts of medicinal particles, 20 parts of potassium nitrate, 12 parts of diammonium phosphate and 20 parts of modified diatomite by mass, and the medicinal particles are prepared in example 6; the preparation steps are as follows: and uniformly stirring the drug particles, the potassium nitrate, the diammonium phosphate and the modified diatomite by using a stirrer to obtain the drug fertilizer.
Comparative example 1: on the basis of example 3, the intermediate product 2 obtained is directly used as a disintegrant without performing the operation of step S3, and the pharmaceutical granules are prepared according to the method of example 6, and then the pharmaceutical fertilizer is prepared according to the method of example 7.
Comparative example 2: a medicinal granule is prepared on the basis of example 6 without adding a disintegrating agent, and then a medicinal fertilizer is prepared according to the method of example 7.
Comparative example 3: a disintegrant was replaced with commercially available low-substituted cellulose on the basis of example 6 to prepare drug granules, and a drug fertilizer was prepared by the method of example 7.
The performance test was performed on example 7 and comparative examples 1 to 3, wherein 60g of each fertilizer was weighed, 12 beakers were taken, 100mL of water was added to each beaker, each fertilizer was divided into three parts and added to the corresponding beakers, the mixture was stirred and timed by a stirrer, the rotation speed was set at 100r/min, the timing was stopped after the fertilizer was completely dissolved, and the average dissolving time (unit is accurate to min) of each fertilizer was calculated, with the results shown in table 1:
TABLE 1
| Item | Example 7 | Comparative example 1 | Comparative example 2 | Comparative example 3 |
| Average dissolution time/min | 6 | 13 | 15 | 12 |
As can be seen from the table 1, the Chinese medicinal fertilizer has better disintegration effect after being added with the disintegrant prepared by the method.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (9)
1. The pesticide fertilizer containing metalaxyl-M and hymexazol for preventing and treating damping off and the application thereof are characterized by comprising the following raw materials in parts by mass: 15-20 parts of drug particles, 18-24 parts of potassium nitrate, 10-15 parts of diammonium phosphate and 18-22 parts of modified diatomite; wherein the drug particles are prepared by the following steps:
the method comprises the following steps: adding metalaxyl-M into a flask, adding sodium dodecyl sulfate and distilled water, magnetically stirring for 15-20min, pretreating beta-cyclodextrin, mixing with the homogeneous emulsion, standing in a water bath for 3-3.5h, and performing aftertreatment to obtain a component A;
step two: adding hymexazol into a flask, adding distilled water, stirring, adding activator and carrageenan, stirring for 25-30min, adding modified resin, stirring, and infrared drying to obtain component B;
step three: mixing the component A, the component B and the disintegrating agent by a stirrer, wetting by absolute ethyl alcohol, and granulating to obtain the medicine granules.
2. The insecticide fertilizer containing metalaxyl-M and hymexazol for preventing and treating damping-off as claimed in claim 1, wherein the drug granules comprise 5-8 parts of component A, 8-10 parts of component B and 3-5 parts of disintegrant by mass.
3. The insecticide fertilizer for preventing and treating damping off, which comprises metalaxyl-M and hymexazol as claimed in claim 1, wherein the step of pretreating in the first step is to dissolve beta-cyclodextrin with distilled water of 70 ℃ in 7 times of volume.
4. The insecticide-fertilizer for preventing and treating damping off containing metalaxyl-M and hymexazol as claimed in claim 1, wherein the activator in step two is edetic acid and tartaric acid in a weight ratio of 7: 4.
5. The metalaxyl-M and hymexazol-containing damping-off controlling medical fertilizer according to claim 1, wherein the disintegrant is prepared by the following steps:
step S1: adding distilled water into a flask, adding lignocellulose, stirring for dissolving, heating to 55-60 ℃, slowly dropwise adding chloroacetic acid solution and sodium hydroxide solution into the solution, controlling the dropwise adding to be finished within 30-35min, carrying out heat preservation reaction for 2-3h, and carrying out post-treatment to obtain an intermediate product 1;
step S2: dissolving the intermediate product 1 with dichloromethane, adding acetic anhydride and silica gel, stirring for dissolving, adding a Sairett reagent, reacting for 45-50min, and performing post-treatment to obtain an intermediate product 2;
step S3: adding sorbitol into a flask, adding an auxiliary agent, magnetically stirring for 20-30min, adding the intermediate product 2 and distilled water, stirring for reacting for 2.5-3.5h, and performing post-treatment to obtain the disintegrating agent.
6. The insecticide fertilizer for preventing and treating rhizoctonia rot, which comprises metalaxyl-M and hymexazol according to claim 5, wherein the dosage ratio of the lignocellulose, the distilled water, the chloroacetic acid and the sodium hydroxide solution in step S1 is 5 g: 100mL of: 75mL:100 mL.
7. The insecticide fertilizer containing metalaxyl-M and hymexazol for preventing and treating damping off as claimed in claim 5, wherein the adjuvant in step S3 is concentrated sulfuric acid, phosphotungstic acid, methanol and dimethyl sulfoxide in a dosage ratio of 8 mL: 0.02 mmol: 35mL of: 20mL of the extract.
8. The insecticide fertilizer containing metalaxyl-M and hymexazol for preventing and treating damping-off as claimed in claim 1, which is prepared by the following steps: and uniformly stirring the drug particles, the potassium nitrate, the diammonium phosphate and the modified diatomite by using a stirrer to obtain the drug fertilizer.
9. The application of the medicinal fertilizer containing metalaxyl-M and hymexazol for preventing and treating damping-off prepared by the method of claim 1 in farmland.
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| CN115340423A (en) * | 2022-08-11 | 2022-11-15 | 赤天化科技集团有限公司 | Pesticide-fertilizer granules for preventing and treating soil-borne diseases of rice seedbed |
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