CN112314596B - Animal-derived acaricide 20-30% amitraz acid water emulsion and preparation method and application thereof - Google Patents
Animal-derived acaricide 20-30% amitraz acid water emulsion and preparation method and application thereof Download PDFInfo
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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
- A01N37/36—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 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
- A01N37/38—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 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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- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
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Abstract
The invention relates to the technical field of biological pesticides, and discloses an animal-derived acaricide 20-30% amitraz acid water emulsion, a preparation method and an application thereof, wherein the emulsion in water comprises the following components in percentage by mass: 20-30% of hexmetryt, 5-8% of solvent, 2-5% of dispersant, 1-5% of emulsifier, 1-4% of co-emulsifier, 0.5-3% of antifreezing agent, 0.2-0.6% of preservative and 44.4-70.3% of deionized water. The hexa-methyl mite acid water emulsion is an animal source acaricide, the original pesticide hexa-methyl mite acid of the hexa-methyl mite acid emulsion is derived from the pupa shell of the yellow moth, and the hexa-methyl mite acid emulsion is low in toxicity, easy to degrade, low in residue, safe to ecological environment and green and safe. The hexaflumuron acid is extracted from the residue of the pupa shell of the yellow spiny moth extracted by petroleum ether, so that the effect of changing waste into valuable is achieved, the hexaflumuron acid water emulsion prepared by the method is one of important means for realizing ecological agriculture and green agriculture, and the hexaflumuron acid water emulsion has wide application prospect in the field of biological pesticides for killing mites.
Description
Technical Field
The invention relates to the technical field of biological pesticides, and particularly relates to an animal-derived acaricide 20-30% amitraz acid water emulsion, and a preparation method and application thereof.
Background
Fa Bu in insect records mentions that the pine moth contacting the skin of the human body causes red swelling, ulceration and itching. However, this irritation to the human skin is not unique to pine moth, and many piercing moths can produce similar responses, even stronger. Such as the lepidopteran insect yellow spiny moth (Cnidocampa flavescens Walker), commonly known as peppery pepper, octagonal nail, etc.
The occurrence of crop mites is extremely serious and is widespread in any crop and region of the world. Among them, commercial crops such as cotton, fruit trees, tea, etc. are the most seriously damaged. Although the mites are small in size, the mites propagate fast, have many generations, are strong in adaptability and easy to generate drug resistance, and are one of the most difficult pest communities to be controlled. The mite can not be effectively controlled in the present and future period of time.
The phytophagous harmful mites are various in species, have the characteristics of small volume, quick propagation, strong adaptability, easy generation of drug resistance and the like, and are about more than 40 species of severely harmful mites, mainly spider mites and gall mites, and severely harm orange trees, apple trees, cotton, vegetables and the like. At present, the acaricide varieties commonly used in China comprise pyridaben, dicofol, spirodiclofen, propargite, abamectin and the like; the main preparation formulation comprises missible oil, microemulsion, aqueous emulsion, microemulsion, suspending agent and the like. Although chemical acaricides such as dicofol have strong acaricidal activity, they have been forbidden due to their serious residues, and the resistance of mites to pyridaben, spirodiclofen, propargite, abamectin, etc. is increasing.
In conclusion, most of the existing acaricides are chemical acaricides, and have the defects of few varieties, single action mechanism, non-ideal acaricidal effect, environmental friendliness and the like, and the acaricides are easy to induce mites to generate drug resistance. Therefore, in order to solve the problems of environmental pollution, drug resistance of mites and the like of chemical acaricides, the acaricides are inevitably developed towards biological pesticides. However, at present, researches on biological acaricides mainly focus on plant sources and microbial sources, few researches on animal acaricides are carried out, and most of the researches on the animal acaricides are nereistoxin insecticides.
Disclosure of Invention
The invention provides a 20-30% hexa-methyl mite acid water emulsion of an animal-derived acaricide, and a preparation method and application thereof. The hexa-methyl-mite acid is extracted from the residue of the yellow moth pupa shell extracted by petroleum ether, so that the method has the benefit of changing waste into valuable, and a large amount of hexa-methyl-mite acid can be obtained by the extraction process. The emulsion in water contains methyl oleate, so that the emulsion in water can avoid the phenomena of flammability and explosiveness in the production, storage and transportation processes, meanwhile, the preparation has no unpleasant and toxic smell, has small irritation to eyes, can reduce environmental pollution, and improves the safety of production, transportation and users.
In order to achieve the technical effects, the technical scheme adopted by the invention is as follows:
an animal source acaricide 20-30% acidum hemsleyanum aqueous emulsion comprises the following components in percentage by mass: 20-30% of hexmetryt, 5-8% of solvent, 2-5% of dispersant, 1-5% of emulsifier, 1-4% of co-emulsifier, 0.5-3% of antifreezing agent, 0.2-0.6% of preservative and 44.4-70.3% of deionized water.
Further, the hexa-methyl mite acid is an active ingredient 3, 5-di-tert-butyl-4-hydroxyphenyl propionic acid which is separated and purified and identified from a yellow moth pupa shell petroleum ether extract species through column chromatography, and has the chemical formula:
the content of the extract in the petroleum ether extract of the pupa shell of the yellow spiny moth is 90.5-98.3%.
Further, the dispersant is any one or two of tween 80, magnesium aluminum silicate, sodium lignin sulfonate, arabic gum and xanthan gum.
Further, the antifreezing agent is one or two of ethylene glycol, propylene glycol, glycerol and urea.
Further, the solvent is methyl oleate.
Further, the emulsifier is one or two of nonionic polyoxyethylene stearate, alkylamide polyoxyethylene ether and ethylene oxide propylene oxide block copolymer.
Further, the coemulsifier is any one or two of butanol, isobutanol and dodecanol.
In order to realize the technical effects, the invention also provides a preparation method of the 20-30% amitraz acid water emulsion of the animal-derived acaricide, which comprises the following steps:
s1, mixing the hexaazapyr and the solvent according to the proportion, fully stirring at normal temperature to completely dissolve the effective components, adding the dispersing agent, the emulsifier, the co-emulsifier and the like, and stirring to form a uniform oil phase;
s2, mixing the antifreezing agent, the preservative and the balance of water, and stirring into a uniform water phase;
and S3, adding the water phase into the oil phase under high-speed stirring, and shearing for 30-40 minutes to emulsify the water phase into a well-dispersed emulsion to obtain the aqueous emulsion.
The application of 20-30% of hexa-methyl mite acid water emulsion of animal-derived acaricide in the field of biological pesticides for killing mites is provided, and mites are mite species of Tetranychus urticae, Tetranychus cinnabarinus, Panonychus citri, Panonychus ulmi, Tetranychus crataegi and Tetranychus camellia sinensis.
The invention has the advantages that:
(1) the animal-derived acaricide of the invention is 20-30% of the hexa-methyl mite acid water emulsion which is an animal-derived acaricide, the original pesticide hexa-methyl mite acid of the hexa-methyl mite acid emulsion is derived from the pupa shell of the yellow moth, the toxicity is low, the hexa-methyl mite acid emulsion is easy to degrade, and the hexa-methyl mite acid emulsion is safe to the ecological environment, and is a green and safe animal-derived acaricide.
(2) The hexa-methyl-mite acid is extracted from the residue of the yellow moth pupa shell extracted by petroleum ether, so that the method has the benefit of changing waste into valuable, and a large amount of hexa-methyl-mite acid can be obtained by the extraction process.
(3) The emulsion in water of the invention only contains methyl oleate, thus being capable of avoiding the phenomena of flammability and explosiveness in the production, storage and transportation processes, simultaneously, the preparation has no bad smell and toxic smell, has small stimulation to eyes, can reduce environmental pollution, and improves the safety of production, transportation and users.
(4) The application of the animal-derived acaricide hexaazapyr in the field of preparation of the acaricidal biopesticides has good application and obvious acaricidal effect, and on one hand, the invention provides a novel animal-derived acaricidal compound to expand the variety of acaricidal substances; on the other hand, the effective utilization way of the yellow spiny moth is increased, and the harm of the yellow spiny moth is reduced.
Detailed Description
Example 1:
an animal source acaricide 20-30% acidum hemsleyanum aqueous emulsion comprises the following components in percentage by mass: 20-30% of hexmetryt, 5-8% of solvent, 2-5% of dispersant, 1-5% of emulsifier, 1-4% of co-emulsifier, 0.5-3% of antifreezing agent, 0.2-0.6% of preservative and 44.4-70.3% of deionized water.
The preparation method comprises the following steps:
s1, mixing the hexaazapyr and the solvent according to the proportion, fully stirring at normal temperature to completely dissolve the effective components, adding the dispersing agent, the emulsifier, the co-emulsifier and the like, and stirring to form a uniform oil phase;
s2, mixing the antifreezing agent, the preservative and the balance of water, and stirring into a uniform water phase;
s3, adding the water phase into the oil phase under high-speed stirring, and shearing for 30-40 minutes to emulsify the water phase into a well-dispersed emulsion to obtain the aqueous emulsion
The hexa-methyl mite acid in the embodiment is obtained from a species extracted from yellow moth pupa shell petroleum ether, the effective component is 3, 5-di-tert-butyl-4-hydroxyphenyl propionic acid, and the chemical formula is as follows:
the content of the extract in the petroleum ether extract of the pupa shell of the yellow spiny moth is 90.5-98.3%.
In this embodiment, the dispersant is any one or two of tween 80, magnesium aluminum silicate, sodium lignosulfonate, gum arabic and xanthan gum. The antifreezing agent is one or two of ethylene glycol, propylene glycol, glycerol and urea. The solvent is methyl oleate. The emulsifier is one or two of nonionic polyoxyethylene stearate, alkylamide polyoxyethylene ether and ethylene oxide propylene oxide block copolymer (Pluronic PE 10500). The coemulsifier is one or two of butanol, isobutanol and dodecanol.
In the embodiment, the acid water emulsion of the hexa-methyl mite is an animal-derived acaricide, the original hexa-methyl mite acid of the hexa-methyl mite acid is derived from the pupa shell of the yellow-moth, and the active ingredient 3, 5-di-tert-butyl-4-hydroxyphenyl propionic acid which is separated, purified and identified from the petroleum ether extract species of the pupa shell of the yellow-moth through column chromatography is low in toxicity, easy to degrade and safe to the ecological environment, so that the hexa-methyl mite acid water emulsion is a green and safe animal-derived acaricide. The hexa-methyl-mite acid is extracted from the residue of the yellow moth pupa shell extracted by petroleum ether, so that the method has the benefit of changing waste into valuable, and a large amount of hexa-methyl-mite acid can be obtained by the extraction process. The emulsion in water contains methyl oleate, so that the emulsion in water can avoid the phenomena of flammability and explosiveness in the production, storage and transportation processes, meanwhile, the preparation has no unpleasant and toxic smell, has small irritation to eyes, can reduce environmental pollution, and improves the safety of production, transportation and users.
The method for extracting the hexa-methyl-mite acid in the embodiment comprises the following steps:
drying pupa Bombycis at 58 deg.C in oven, pulverizing with high speed pulverizer, mixing the pulverized material with petroleum ether (60-90 deg.C) at a certain ratio (v/w is 5:1), placing into wide-mouth bottle, standing, and stirring periodically. Filtering the extract with a filter device, and performing rotary steaming and concentration to obtain the yellow moth pupa shell petroleum ether extract. Mixing 4.0g extract with 4.0g activated silica gel, laying a layer of quartz sand on the top layer of the filled silica gel column, and carefully placing the mixture of extract and silica gel. Petroleum ether-ethyl acetate (20:1(500mL),15:1(500mL),10:1(500mL),7:1(500mL),5:1(500mL),1:1(500mL), v/v)) was used as an eluent to perform gradient elution, silica gel G (200 mesh) 250G was used as a stationary phase, and a fraction was collected at a flow rate of 2 drops/s and 200 mL. The same fractions were combined, concentrated to dryness under reduced pressure and stored separately by TLC (developing solvent: petroleum ether: ethyl acetate ═ 6:1, v/v) and observed under uv light at 254nm and 365 nm. The obtained component 2 is further separated and purified, and the molecular formula of the substance is identified to be C by combining modern analysis and determination technologies such as element analysis, UV, IR, MS and the like17H26O3Molecular weight is 278, chemical name: 3, 5-di-tert-butyl-4-hydroxyphenylpropionic acid. The general name of the pesticide is named as hexameclofenac by the national pesticide standardization technical committee (2020) agricultural standard character No. 027.
The application of the animal-derived acaricide hexaazapyr in the field of preparation of the miticidal biopesticides has good application and remarkable miticidal effect, and on one hand, the animal-derived acaricide compound is provided, so that the variety of miticidal substances is expanded; on the other hand, the effective utilization way of the yellow spiny moth is increased, and the harm of the yellow spiny moth is reduced.
Example 2:
an animal source acaricidal active substance 20-30% hexa-methyl mite acid water emulsion comprises 20% hexa-methyl mite acid, 5% methyl oleate solvent, 2% tween 80 dispersant, 2% glycol antifreeze, 2% polyoxyethylene stearate emulsifier, 1% butanol co-emulsifier and 68% deionized water.
Example 3:
an animal source acaricidal active substance 20-30% hexa-methyl mite acid water emulsion comprises hexa-methyl mite acid 25%, methyl oleate 6%, magnesium aluminum silicate dispersant 2%, propylene glycol antifreeze 2%, alkyl amide polyoxyethylene ether emulsifier 2%, isobutanol co-emulsifier 1% and deionized water 62%.
Example 4:
an animal source acaricidal active substance 20-30% hexa-methyl mite acid water emulsion is composed of hexa-methyl mite acid 30%, methyl oleate solvent 8%, magnesium aluminum silicate dispersant 4%, glycerin antifreezing agent 2%, ethylene oxide propylene oxide block copolymer Pluronic PE10500 emulsifier 2%, isobutanol 3% co-emulsifier and deionized water 51%.
Example 5:
an animal source acaricidal active substance 20-30% hexa-methyl mite acid water emulsion is composed of hexa-methyl mite acid 28%, methyl oleate solvent 6%, acacia gum dispersing agent 4%, urea antifreezing agent 2%, alkylamide polyoxyethylene ether 3%, isobutanol 3% co-emulsifier and deionized water 54%.
Example 6:
the results of comparing the biological activities of the two to tetranychus cinnabarinus when the content of the six-methyl-mite-acid is different are shown in table 1, and it can be seen that the biological activities are better when the content of the six-methyl-mite-acid is 20-30%.
TABLE 1 comparison of the biological activities of different contents of water emulsions of carmine spider mite against Tetranychus cinnabarinus (0.25 mg. mL)-1，48h)
The field efficacy test refers to GB/T17980.74-2004 part 74 of pesticide field efficacy test criteria (II): the pesticide is used for preventing and treating cotton red spider. Inoculating Tetranychus cinnabarinus bred indoors to unopened cotton leaves planted in test field of plant protection garden of southwest university, and after the leaves are propagated to a certain amount, dividing the cotton field into small zones with area of 20m2The test agent, control agent and blank control cells were treated with cotton in random block arrays, with 1m spacing between each cell. Each treatment was repeated 3 times, and 10 cotton leaves were planted and listed in each plot.
The application was carried out using a conventional gongnong-16 type knapsack sprayer, and the number of mites treated before application was investigated and the number of mites after application was investigated 7d and 15 d. After the test is finished, the decline rate and the control effect of each treatment are calculated according to the number of the mites before and after the treatment. As can be seen from the table 2, the 25% acidum hexaflumorphum acid water emulsion has very excellent field control effect on tetranychus cinnabarinus, and the three liquid medicines with diluted concentrations can effectively control tetranychus cinnabarinus 15 days after application, and the control effect is more than 98%.
TABLE 225% aqueous emulsion of Tetranychus urticae followed by 7d and 15d field effects on Tetranychus cinnabarinus
The above is an embodiment of the present invention. The embodiments and specific parameters in the embodiments are only for the purpose of clearly illustrating the process of verifying the invention and are not intended to limit the scope of the invention, which is defined by the claims, and all the equivalent structural changes made by applying the content of the specification of the invention should be covered by the scope of the invention.
Claims (7)
1. The animal source acaricide acid aqueous emulsion with 20-30% of amitraz is characterized in that the aqueous emulsion comprises the following components in percentage by mass: 20-30% of hexamanthalic acid, 5-8% of solvent, 2-5% of dispersant, 1-5% of emulsifier, 1-4% of co-emulsifier, 0.5-3% of antifreezing agent, 0.2-0.6% of preservative and 44.4-70.3% of deionized water; the solvent is methyl oleate;
the hexa-methyl acarinic acid is an active ingredient 3, 5-di-tert-butyl-4-hydroxyphenyl propionic acid which is separated and purified by column chromatography from a petroleum ether extract species of a pupa shell of a yellow moth and identified, and has the chemical formula:
the content of the extract in the petroleum ether extract of the pupa shell of the yellow spiny moth is 90.5-98.3%.
2. The animal-derived acaricide of claim 1, which is 20-30% aqueous emulsion of water containing amitraz, characterized in that: the dispersant is any one or two of tween 80, magnesium aluminum silicate, sodium lignosulfonate, arabic gum and xanthan gum.
3. The animal-derived acaricide of claim 1, which is 20-30% aqueous emulsion of water containing amitraz, characterized in that: the antifreezing agent is one or two of ethylene glycol, propylene glycol, glycerol and urea.
4. The animal-derived acaricide of claim 1, which is 20-30% aqueous emulsion of water containing amitraz, characterized in that: the emulsifier is one or two of nonionic polyoxyethylene stearate, alkylamide polyoxyethylene ether and ethylene oxide propylene oxide block copolymer.
5. The animal-derived acaricide of claim 1, which is 20-30% aqueous emulsion of water containing amitraz, characterized in that: the coemulsifier is any one or two of butanol, isobutanol and dodecanol.
6. A method for preparing 20-30% aqueous emulsion of water containing spider mites of an animal-derived miticide, which is used for preparing 20-30% aqueous emulsion of water containing spider mites of any one of claims 1-5, and which comprises: the method comprises the following steps:
s1, mixing the hexaazapyr and the solvent according to the proportion, fully stirring at normal temperature to completely dissolve the effective components, adding the dispersant, the emulsifier and the co-emulsifier, and stirring into a uniform oil phase;
s2, mixing the antifreezing agent, the preservative and the balance of water, and stirring into a uniform water phase;
and S3, adding the water phase into the oil phase under high-speed stirring, and shearing for 30-40 minutes to emulsify the water phase into a well-dispersed emulsion to obtain the aqueous emulsion.
7. The use of 20-30% water emulsion of hexa-methyl mite acid of animal-derived acaricide prepared in claim 6 in the field of biological pesticides for killing mites is characterized in that: the mite is spider mite, including Tetranychus urticae, Tetranychus cinnabarinus, Panonychus citri, Panonychus ulmi, Tetranychus viennensis and Tetranychus camellia.
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