CN106818726A - A kind of emamectin-benzoate mite killing suspending agent for suppressing mite egg hatching and preparation method thereof - Google Patents
A kind of emamectin-benzoate mite killing suspending agent for suppressing mite egg hatching and preparation method 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
- 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
- A01N25/08—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 solids as carriers or diluents
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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
- A01N43/90—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having two or more relevant hetero rings, condensed among themselves or with a common carbocyclic ring system
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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
- A01N65/00—Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof
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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
- A01N65/00—Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof
- A01N65/08—Magnoliopsida [dicotyledons]
- A01N65/26—Meliaceae [Chinaberry or Mahogany family], e.g. mahogany, langsat or neem
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Abstract
A kind of emamectin-benzoate mite killing suspending agent for suppressing mite egg hatching, it is characterised in that it is prepared from by following raw material：Emamectin benzoate, methyl alcohol, phosphoric acid solution, toluene, isopropyl acetate, castor oil polyester vinyl ether, benzoic acid, n-hexane, neem seed, tea seed, dichloromethane, ethyl acetate, calcium chloride, acetone, shitosan, acetic acid, polysorbate, atoleine, vanillic aldehyde, glutaraldehyde, triphenyl phosphate, polyoxyethylene octadecanol, salicylic acid, appropriate deionized water.Mite killing suspending agent of the invention can efficiently lure acarid, acarid is effectively killed, with excellent synergistic effect, acaricidal field dosage is reduced, residues of pesticides and the harm to beneficial organism can be effectively reduced, while reducing cost accounting and mitigating the pollution to environment.
Description
Technical field
The invention belongs to agricultural pesticide field, and in particular to a kind of emamectin benzoate benzoic acid of suppression mite egg hatching
Salt mite killing suspending agent and preparation method thereof.
Background technology
It is current main to use chemical pesticide control agricultural pest, but over time, the drawbacks of chemical pesticide by
Gradually it is exposed, of particular concern is the rampant and resistance problem mad again of residues of pesticides, insect, these problems promotes people to open
Beginning finds the substitute of chemical pesticide.AVM is that antibioticses desinsection kills full mite agent, belongs to biological source insecticide, with chemistry
Unlike agricultural chemical insecticide, AVM mainly by disturbing insect nervous physiology activity, stimulates release GABA,
And aminobutyric acid has inhibitory action to the nerve conduction of arthropod, mite class adult, nymph and insect larvae and AVM connect
There is paralysis symptom after touch, inertia, do not take food, it is dead after 2~4 days.AVM is to insect predator and insect parasite
Though there is direct action of contace poison, because plant surface residual is few, therefore to the damage very little of beneficial insect.AVM is in soil by soil
Absorption will not be moved, and can be decomposed by the microorganisms, thus in the environment without cumulative function.Due to not causing insect to take off rapidly
Water, AVM lethal effect is more slow.
Author Chen Fuliang exists《The development of the avermectin micro-emulsion containing organosilicon auxiliary agent》In one text, with 7% Avermectin
Element, 6% cyclohexanone, 4% dimethyl sulfoxide (DMSO), 5% organosilicon auxiliary agent Silwet408 and balance of water, are obtained AVM micro-
Emulsion；Addition organosilicon auxiliary agent can not only significantly reduce liquid surface tension and improve liquid blade surface wetting,
Ability is opened up, increases the expanding area of liquid, and liquid can be made to enter hidden close insect hiding place, and promote plant leaf surface pair
The absorption of active ingredient and enter epidermis, extend its lasting period；But active ingredient is single Avermectin in the microemulsion
Element, its Insecticiding-miticiding is inefficient, and lethal effect is slow.
The content of the invention
It is an object of the invention to provide the emamectin benzoate benzene first of a kind of efficient and lasting suppression mite egg hatching
Hydrochlorate mite killing suspending agent and preparation method thereof.
To achieve these goals, the present invention is adopted the following technical scheme that：
A kind of emamectin-benzoate mite killing suspending agent for suppressing mite egg hatching, it is characterised in that it by weighing as follows
The raw material for measuring part is prepared from：Emamectin benzoate 6-8 parts, methyl alcohol 120-150 parts, phosphoric acid solution 30-40 parts, toluene 200-
250 parts, isopropyl acetate 60-70 parts, 2-3 parts of castor oil polyester vinyl ether, benzoic acid 12-15 parts, n-hexane 180-200 parts,
Neem seed 6-8 parts, tea seed 5-6 parts, dichloromethane 80-100 parts, ethyl acetate 50-60 parts, calcium chloride 5-6 parts, acetone
80-100 parts, shitosan 18-20 parts, acetic acid 4-5 parts, polysorbate 2-3 parts, atoleine 80-100 parts, vanillic aldehyde 4-5 parts,
Glutaraldehyde 3-4 parts, triphenyl phosphate 0.5-1 parts, polyoxyethylene octadecanol 2-3 parts, salicylic acid 3-4 parts, appropriate deionized water.
The emamectin-benzoate mite killing suspending agent of described suppression mite egg hatching, it is characterised in that its by
Following steps are prepared from：
（1）At room temperature, emamectin benzoate is added in 2/3 methyl alcohol, is stirred to being completely dissolved, be slowly added dropwise phosphoric acid molten
The mixed solution that liquid is configured with remaining methyl alcohol, continues to mix 1-2h after completion of dropping；1/2 toluene is added, continues mixed
Conjunction stirring 1-2h, is transferred them in ice-water bath, continues to mix 5-6h, and centrifugation, precipitation is used and pre-cooled to 0 DEG C
Remaining toluene wash 2-3 time, be vacuum dried；Product after vacuum drying is added to equivalent to emamectin benzoate weight
Measure in the deionized water of 3-4 times of part, stirring dissolves it, add isopropyl acetate, regulation system PH is 8-9, mixes 30-
3-4h is stood after 40min, organic phase is separated；Castor oil polyester vinyl ether is added in organic phase, stirring makes it fully dissolve,
Benzoic acid is added at room temperature, reaction 5-6h is mixed, 1/2 n-hexane is slowly added dropwise, and continues to mix after completion of dropping
Reaction 4-5h, filtering, filter cake is washed 2-3 times with remaining n-hexane, is vacuum dried, and obtains emamectin benzoate benzoic acid
Salt；
（2）By neem seed and the cold slag oil removing of shelling camellia seeds；Oil cake after will be fuel-displaced is using dichloromethane in 40-45 DEG C of temperature
Condition, under conditions of ultrasonic power 300-400W, carries out ultrasound assisted extraction 40-50min, filtering, collects filtrate；Filter cake is again
In microwave power it is 650-700w, microwave abstracting 50-60min with ethyl acetate, filtrate is collected in filtering；Merging filtrate, 40-50
DEG C concentrate and be vacuum dried；
（3）By step（1）Product, step（2）Product, calcium chloride be added in 2/3 acetone, after mixing and stirring,
It is slowly added into shitosan, acetic acid and the solution that is configured equivalent to the deionized water of 30-35 times of acetic acid weight portion, mixes
After uniform, the solution of polysorbate and atoleine configuration is added to ,/min is turned with 2200-2500 in 50-55 DEG C of water-bath
Rotating speed constant temperature quickly stir 25-30min, form white " milky " liquid, lead to nitrogen 20-30min, add vanillic aldehyde, glutaraldehyde
The solution configured with remaining acetone, 65-70 DEG C is continued to stir 5-6h, is washed with deionized 2-3 times, centrifugation, 60-65
20-24h is dried in DEG C vacuum drying chamber, obtains loading the chitosan sustained-release microsphere of emamectin-benzoate；
（4）By step（3）Product, triphenyl phosphate is added to equivalent to step（3）Products weight part 15-20 times go from
In sub- water, ultrasonic disperse 30-40min adds polyoxyethylene octadecanol, salicylic acid, is stirred with the rotating speed of 800-1000 turns/min
25-30min is mixed, the emamectin-benzoate mite killing suspending agent of the mite egg hatching that is inhibited.
The emamectin-benzoate mite killing suspending agent of described suppression mite egg hatching, it is characterised in that described
Phosphoric acid solution concentration be 0.5-0.6mol/L.
Beneficial effects of the present invention are：
The present invention is main acaricide with emamectin-benzoate, and compared to AVM parent, it is to Lepidoptera elder brother
The activity of worm larva is generally improved, and is especially 6 times of AVM to the preventing and treating of acarid；Emamectin-benzoate
Belong to biogenic pesticide, with its unique mechanism of action, be difficult to remain, can be biodegradable, it is safe and environment-friendly the advantages of, meet
Develop the requirement of nuisanceless fruits and vegetables, pollution-free food；The extract of present invention addition neem seed and tea seed, with methylamino AVM hereinafter
Rhzomorph benzoate is acted synergistically, and nimbin, bitter principle and Tea Polyphenols isoreactivity material are rich in extract, and nimbin being capable of shadow
Acarid internal system is rung, the hormone regulating and controlling of Oogenesis is disturbed, influences Oogenesis, Tea Polyphenols that there are spectrum bactericidal properties
Can, pathogen can be killed；The present invention wraps up AVM using shitosan, and shitosan is handed over using vanillic aldehyde and glutaraldehyde
Connection, obtains sustained-release micro-spheres, can not only slow release medicine, extend the service life of medicament, it can be significantly reduced and stored
Middle resolution ratio, and shitosan can promote medicament to be absorbed by plants rapidly through Stoma of Leaves, further increase miticidal effect；This hair
Bright mite killing suspending agent can efficiently lure acarid, effectively kill acarid, with excellent synergistic effect, reduce acaricidal field
Between dosage, can effectively reduce residues of pesticides and the harm to beneficial organism, at the same reduce cost accounting and mitigate to environment
Pollution.
Specific embodiment
The emamectin-benzoate mite killing suspending agent of the suppression mite egg hatching of the present embodiment, it is by following weight
The raw material of part is prepared from：8 parts of emamectin benzoate, 150 parts of methyl alcohol, 40 parts of phosphoric acid solution, 250 parts of toluene, isopropyl acetate
70 parts of ester, 3 parts of castor oil polyester vinyl ether, 15 parts of benzoic acid, 200 parts of n-hexane, 7 parts of neem seed, 6 parts of tea seed, dichloro
100 parts of methane, 60 parts of ethyl acetate, 6 parts of calcium chloride, 100 parts of acetone, 20 parts of shitosan, 5 parts of acetic acid, 3 parts of polysorbate, liquid
80 parts of body paraffin, 5 parts of vanillic aldehyde, 3 parts of glutaraldehyde, 1 part of triphenyl phosphate, 3 parts of polyoxyethylene octadecanol, 4 parts of salicylic acid, go
Ion appropriate amount of water.
The emamectin-benzoate mite killing suspending agent of the suppression mite egg hatching of the present embodiment, it is by following steps
It is prepared from：
（1）At room temperature, emamectin benzoate is added in 2/3 methyl alcohol, is stirred to being completely dissolved, be slowly added dropwise phosphoric acid molten
The mixed solution that liquid is configured with remaining methyl alcohol, continues to mix 2h after completion of dropping；1/2 toluene is added, continues to mix
Stirring 2h, is transferred them in ice-water bath, continues to mix 6h, and centrifugation, precipitation is used and pre-cooled to 0 DEG C of residue
Toluene wash 3 times, vacuum drying；Product after vacuum drying is added to equivalent to 4 times of emamectin benzoate weight portion
Deionized water in, stirring dissolve it, add isopropyl acetate, regulation system PH be 8-9, mix 40min after stand
4h, separates organic phase；Castor oil polyester vinyl ether is added in organic phase, stirring makes it fully dissolve, and benzene is added at room temperature
Formic acid, mixes reaction 6h, is slowly added dropwise 1/2 n-hexane, continues to mix reaction 5h, filtering, filter after completion of dropping
Cake is washed 3 times with remaining n-hexane, vacuum drying, obtains emamectin-benzoate；
（2）By neem seed and the cold slag oil removing of shelling camellia seeds；Oil cake after will be fuel-displaced is using dichloromethane in temperature 45 C bar
Part, under conditions of ultrasonic power 400W, carries out ultrasound assisted extraction 50min, filtering, collects filtrate；Filter cake uses acetic acid second again
Ester is 650w, microwave abstracting 60min in microwave power, and filtrate is collected in filtering；Merging filtrate, 50 DEG C concentrate and are vacuum dried；
（3）By step（1）Product, step（2）Product, calcium chloride be added in 2/3 acetone, after mixing and stirring,
It is slowly added into shitosan, acetic acid and the solution that is configured equivalent to the deionized water of 35 times of acetic acid weight portion, mixes equal
After even, the solution of polysorbate and atoleine configuration is added to, with the rotating speed constant temperature of 2500 turns/min in 55 DEG C of water-baths
Quick stirring 30min, forms white " milky " liquid, leads to nitrogen 30min, adds the configuration of vanillic aldehyde, glutaraldehyde and remaining acetone
Solution, 70 DEG C continue stir 6h, be washed with deionized 3 times, centrifugation, dry 24h in 65 DEG C of vacuum drying chambers, obtain
Load the chitosan sustained-release microsphere of emamectin-benzoate；
（4）By step（3）Product, triphenyl phosphate is added to equivalent to step（3）Products weight parts 20 times deionization
In water, ultrasonic disperse 40min adds polyoxyethylene octadecanol, salicylic acid, and 30min is stirred with the rotating speed of 1000 turns/min, obtains
To the emamectin-benzoate mite killing suspending agent for suppressing mite egg hatching.
Test method：Caught from field and come each 200 of cabbage caterpillar, heart-eating worm, vegetable aphid, planthopper, acarid, every kind of insect
Individually it is placed in plastic tub, the dish leaf 2 of equivalent is put into each plastic tub, by the mite killing suspending agent dilute with water of the present embodiment
500 times, then the mite killing suspending agent after dilution is uniformly sprayed in plastic tub, dish leaf is stirred during sprinkling, make its comprehensively medicine,
Plastic tub bottom retains without liquid, then covers plastic tub with gauze and seals, and then the insect of 24h and 48h is dead after statistics spray
Die rate.
Result of the test：
| The death rate after spray 24h | The death rate after spray 48h | |
| Cabbage caterpillar | 81.2% | 88.5% |
| Heart-eating worm | 83.6% | 89.1% |
| Vegetable aphid | 85.4% | 93.4% |
| Planthopper | 83.5% | 91.4% |
| Acarid | 93.2% | 99.2% |
Claims (3)
1. it is a kind of suppress mite egg hatching emamectin-benzoate mite killing suspending agent, it is characterised in that it is by as follows
The raw material of weight portion is prepared from：Emamectin benzoate 6-8 parts, methyl alcohol 120-150 parts, phosphoric acid solution 30-40 parts, toluene
200-250 parts, isopropyl acetate 60-70 parts, 2-3 parts of castor oil polyester vinyl ether, benzoic acid 12-15 parts, n-hexane 180-200
Part, neem seed 6-8 parts, tea seed 5-6 parts, dichloromethane 80-100 parts, ethyl acetate 50-60 parts, calcium chloride 5-6 parts, third
Ketone 80-100 parts, shitosan 18-20 parts, acetic acid 4-5 parts, polysorbate 2-3 parts, atoleine 80-100 parts, vanillic aldehyde 4-5
Part, glutaraldehyde 3-4 part, triphenyl phosphate 0.5-1 parts, polyoxyethylene octadecanol 2-3 parts, salicylic acid 3-4 parts, deionized water it is suitable
Amount.
2. according to claims 1 suppression mite egg hatching emamectin-benzoate mite killing suspending agent, its
It is characterised by, it is prepared from by following steps：
（1）At room temperature, emamectin benzoate is added in 2/3 methyl alcohol, is stirred to being completely dissolved, be slowly added dropwise phosphoric acid molten
The mixed solution that liquid is configured with remaining methyl alcohol, continues to mix 1-2h after completion of dropping；1/2 toluene is added, continues mixed
Conjunction stirring 1-2h, is transferred them in ice-water bath, continues to mix 5-6h, and centrifugation, precipitation is used and pre-cooled to 0 DEG C
Remaining toluene wash 2-3 time, be vacuum dried；Product after vacuum drying is added to equivalent to emamectin benzoate weight
Measure in the deionized water of 3-4 times of part, stirring dissolves it, add isopropyl acetate, regulation system PH is 8-9, mixes 30-
3-4h is stood after 40min, organic phase is separated；Castor oil polyester vinyl ether is added in organic phase, stirring makes it fully dissolve,
Benzoic acid is added at room temperature, reaction 5-6h is mixed, 1/2 n-hexane is slowly added dropwise, and continues to mix after completion of dropping
Reaction 4-5h, filtering, filter cake is washed 2-3 times with remaining n-hexane, is vacuum dried, and obtains emamectin benzoate benzoic acid
Salt；
（2）By neem seed and the cold slag oil removing of shelling camellia seeds；Oil cake after will be fuel-displaced is using dichloromethane in 40-45 DEG C of temperature
Condition, under conditions of ultrasonic power 300-400W, carries out ultrasound assisted extraction 40-50min, filtering, collects filtrate；Filter cake is again
In microwave power it is 650-700w, microwave abstracting 50-60min with ethyl acetate, filtrate is collected in filtering；Merging filtrate, 40-50
DEG C concentrate and be vacuum dried；
（3）By step（1）Product, step（2）Product, calcium chloride be added in 2/3 acetone, after mixing and stirring,
It is slowly added into shitosan, acetic acid and the solution that is configured equivalent to the deionized water of 30-35 times of acetic acid weight portion, mixes
After uniform, the solution of polysorbate and atoleine configuration is added to ,/min is turned with 2200-2500 in 50-55 DEG C of water-bath
Rotating speed constant temperature quickly stir 25-30min, form white " milky " liquid, lead to nitrogen 20-30min, add vanillic aldehyde, glutaraldehyde
The solution configured with remaining acetone, 65-70 DEG C is continued to stir 5-6h, is washed with deionized 2-3 times, centrifugation, 60-65
20-24h is dried in DEG C vacuum drying chamber, obtains loading the chitosan sustained-release microsphere of emamectin-benzoate；
（4）By step（3）Product, triphenyl phosphate is added to equivalent to step（3）Products weight part 15-20 times go from
In sub- water, ultrasonic disperse 30-40min adds polyoxyethylene octadecanol, salicylic acid, is stirred with the rotating speed of 800-1000 turns/min
25-30min is mixed, the emamectin-benzoate mite killing suspending agent of the mite egg hatching that is inhibited.
3. according to claims 1,2 suppression mite egg hatching emamectin-benzoate mite killing suspending agent,
Characterized in that, the concentration of described phosphoric acid solution is 0.5-0.6mol/L.
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| CN201611202581.2A CN106818726A (en) | 2016-12-23 | 2016-12-23 | A kind of emamectin-benzoate mite killing suspending agent for suppressing mite egg hatching and preparation method thereof |
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Cited By (1)
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|---|---|---|---|---|
| CN117426400A (en) * | 2023-12-20 | 2024-01-23 | 中科生物技术(山东)有限公司 | Synergistic auxiliary agent of acaricide, preparation method and application thereof |
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2016
- 2016-12-23 CN CN201611202581.2A patent/CN106818726A/en not_active Withdrawn
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117426400A (en) * | 2023-12-20 | 2024-01-23 | 中科生物技术(山东)有限公司 | Synergistic auxiliary agent of acaricide, preparation method and application thereof |
| CN117426400B (en) * | 2023-12-20 | 2024-03-29 | 中科生物技术(山东)有限公司 | Synergistic auxiliary agent of acaricide, preparation method and application thereof |
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Application publication date: 20170613 |