CN106857569A - A kind of emamectin-benzoate mite killing suspending agent of photoactivation synergy and preparation method thereof - Google Patents
A kind of emamectin-benzoate mite killing suspending agent of photoactivation synergy and preparation method thereof Download PDFInfo
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- CN106857569A CN106857569A CN201611202639.3A CN201611202639A CN106857569A CN 106857569 A CN106857569 A CN 106857569A CN 201611202639 A CN201611202639 A CN 201611202639A CN 106857569 A CN106857569 A CN 106857569A
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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
- 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
- A01N43/02—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms
- A01N43/04—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom
- A01N43/14—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom six-membered rings
- A01N43/16—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom six-membered rings with oxygen as the ring hetero atom
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Abstract
The emamectin-benzoate mite killing suspending agent of a kind of photoactivation synergy, it is characterised in that it is prepared from by following raw material：Emamectin benzoate, methyl alcohol, phosphoric acid solution, toluene, isopropyl acetate, t-butyl methyl ether, benzoic acid, n-hexane, 4 Hydroxycoumarins, dichloromethane, phenylacetaldehyde, cyclopentanone, nitromethane, triphenylphosphine, ethyl acetate, nano-calcium carbonate, isopropyl three (dioctylphyrophosphoric acid acyloxy) titanate esters, acetone, stearic acid, HMPA, sodium carboxymethylcellulose, polyoxyethylene octadecanol, ethylene glycol, appropriate saturated sodium bicarbonate aqueous solution, 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 of photoactivation synergy
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 benzoic acid of a kind of efficient and lasting photoactivation synergy
Salt mite killing suspending agent and preparation method thereof.
To achieve these goals, the present invention is adopted the following technical scheme that：
The emamectin-benzoate mite killing suspending agent of a kind of photoactivation synergy, it is characterised in that it is by following weight
The raw material of 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, t-butyl methyl ether 2-3 parts, benzoic acid 12-15 parts, n-hexane 180-200 parts, 4- hydroxyls
Butylcoumariii 5-6 parts, dichloromethane 80-100 parts, phenylacetaldehyde 3-4 parts, cyclopentanone 6-8 parts, nitromethane 20-25 parts, triphenyl
Phosphine 1-1.5 parts, ethyl acetate 30-35 parts, nano-calcium carbonate 30-35 parts, isopropyl three (dioctylphyrophosphoric acid acyloxy) metatitanic acid
Ester 2-3 parts, acetone 80-100 parts, stearic acid 3-4 parts, HMPA 0.5-1 parts, sodium carboxymethylcellulose 1-2 parts, ten
Eight 2-3 parts of alcohol APEOs, ethylene glycol 3-4 parts, appropriate saturated sodium bicarbonate aqueous solution, appropriate deionized water.
The emamectin-benzoate mite killing suspending agent of described photoactivation synergy, it is characterised in that it is by such as
Lower step 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 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；T-butyl methyl ether is added in organic phase, stirring makes it fully dissolve, room temperature
Lower addition benzoic acid, mixes reaction 5-6h, is slowly added dropwise 1/2 n-hexane, continues to mix reaction after completion of dropping
4-5h, filtering, filter cake is washed 2-3 times with remaining n-hexane, is vacuum dried, and obtains emamectin-benzoate；
（2）4 hydroxy coumarin, dichloromethane are added in reaction vessel, after mixing and stirring, phenylacetaldehyde and ring is added
Pentanone, continues mixing and stirring, adds nitromethane and triphenylphosphine, and reaction 8-10h is mixed at room temperature, filters,
Filter cake is added in ethyl acetate, mix 50-60min, using saturated sodium bicarbonate aqueous solution wash to solution substantially without
Color, vacuum distillation removes ethyl acetate, and recrystallization obtains modified furocoumarin compound；
（3）Nano-calcium carbonate is added in high-speed mixer, heat temperature raising stirring treats that temperature reaches 100-105 DEG C, and mixing is stirred
Mix 8-10min；By isopropyl three (dioctylphyrophosphoric acid acyloxy) titanate esters, step（1）Product, step（2）Product and
The solution of acetone configuration is sprayed on calcium carbonate while stirring, rises high-temperature to 120-130 DEG C, continues to mix 15-
20min, adds stearic acid, continues to stir mixing 18-20min；By material in 100-110 DEG C of discharge high-speed mixer, cool down,
It is standby
（4）By step（3）Product, HMPA, sodium carboxymethylcellulose be added to equivalent to step（3）Product
In the deionized water of 15-20 times of weight portion, ultrasonic disperse 30-40min adds polyoxyethylene octadecanol, ethylene glycol, with 800-
The rotating speed stirring 25-30min of 1000 turns/min, the emamectin-benzoate mite killing for obtaining photoactivation synergy suspends
Agent.
The emamectin-benzoate mite killing suspending agent of described photoactivation synergy, it is characterised in that described
The concentration of phosphoric acid solution is 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；Present invention addition cumarin, and it is modified to it using phenylacetaldehyde and cyclopentanone,
With emamectin-benzoate synergy, modified cumarin not only under light illumination can be into hundred times of ground raisings to evil
Worm, evil mite, the lethality of worm's ovum, and to person poultry harmless, it is easily decomposes in the environment；The present invention first adopts nano-calcium carbonate
With titanate coupling agent modified, then by emamectin benzoate benzene first salt and the absorption of modified cumarin, be supported on modified Nano carbon
On sour calcium, can not only slow release medicine, extend the service life of medicament, its resolution ratio in storage can be significantly reduced,
And titanate coupling agent and sodium carboxymethylcellulose can promote medicament to be attached on plant base of leaf, be inhaled by plant rapidly
Receive, further increase miticidal effect；Mite killing suspending agent of the invention can efficiently lure acarid, acarid effectively be killed, with excellent
Synergistic effect, reduce acaricidal field dosage, can effectively reduce residues of pesticides and the harm to beneficial organism, together
When reduce cost accounting and mitigate pollution to environment.
Specific embodiment
The emamectin-benzoate mite killing suspending agent of the photoactivation synergy of the present embodiment, it is by following weight portion
Raw material be 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, 3 parts of t-butyl methyl ether, 15 parts of benzoic acid, 200 parts of n-hexane, 6 parts of 4 hydroxy coumarin, 100 parts of dichloromethane, benzene
4 parts of acetaldehyde, 8 parts of cyclopentanone, 25 parts of nitromethane, 1.5 parts of triphenylphosphine, 35 parts of ethyl acetate, 35 parts of nano-calcium carbonate, isopropyl
3 parts of base three (dioctylphyrophosphoric acid acyloxy) titanate esters, 100 parts of acetone, 4 parts of stearic acid, 1 part of HMPA, carboxylic first
2 parts of base sodium cellulosate, 3 parts of polyoxyethylene octadecanol, 4 parts of ethylene glycol, appropriate saturated sodium bicarbonate aqueous solution, deionized water are fitted
Amount.
The emamectin-benzoate mite killing suspending agent of the photoactivation synergy of the present embodiment, it is by following steps system
It is standby to form：
（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 9, mix 40min after stand 4h,
Separate organic phase；T-butyl methyl ether is added in organic phase, stirring makes it fully dissolve, and benzoic acid is added at room temperature, mixed
Stirring reaction 6h is closed, 1/2 n-hexane is slowly added dropwise, continues to mix reaction 5h after completion of dropping, filtering, filter cake is remaining
N-hexane wash 3 times, vacuum drying, obtain emamectin-benzoate；
（2）4 hydroxy coumarin, dichloromethane are added in reaction vessel, after mixing and stirring, phenylacetaldehyde and ring is added
Pentanone, continues mixing and stirring, adds nitromethane and triphenylphosphine, and reaction 10h, filtering, filter are mixed at room temperature
Cake is added in ethyl acetate, mixes 60min, washs substantially colorless to solution using saturated sodium bicarbonate aqueous solution, is subtracted
Pressure is distilled off ethyl acetate, recrystallizes, and obtains modified furocoumarin compound；
（3）Nano-calcium carbonate is added in high-speed mixer, heat temperature raising stirring treats that temperature reaches 105 DEG C, mixes
10min；By isopropyl three (dioctylphyrophosphoric acid acyloxy) titanate esters, step（1）Product, step（2）Product and acetone
The solution of configuration is sprayed on calcium carbonate while stirring, rises high-temperature to 130 DEG C, continues to mix 20min, adds tristearin
Acid, continues to stir mixing 20min；By material in 110 DEG C of discharge high-speed mixers, cooling is standby
（4）By step（3）Product, HMPA, sodium carboxymethylcellulose be added to equivalent to step（3）Product
In the deionized water that 20 times of weight portion, ultrasonic disperse 40min adds polyoxyethylene octadecanol, ethylene glycol, with 1000 turns/min
Rotating speed stirring 30min, obtain the emamectin-benzoate mite killing suspending agent of photoactivation synergy.
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 | 88.1% | 95.6% |
| Heart-eating worm | 82.4% | 91.4% |
| Vegetable aphid | 83.5% | 93.5% |
| Planthopper | 81.5% | 92.4% |
| Acarid | 91.3% | 98.6% |
Claims (3)
1. the emamectin-benzoate mite killing suspending agent of a kind of photoactivation synergy, 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, t-butyl methyl ether 2-3 parts, benzoic acid 12-15 parts, n-hexane 180-200 parts, 4- hydroxyls
Butylcoumariii 5-6 parts, dichloromethane 80-100 parts, phenylacetaldehyde 3-4 parts, cyclopentanone 6-8 parts, nitromethane 20-25 parts, triphenyl
Phosphine 1-1.5 parts, ethyl acetate 30-35 parts, nano-calcium carbonate 30-35 parts, isopropyl three (dioctylphyrophosphoric acid acyloxy) metatitanic acid
Ester 2-3 parts, acetone 80-100 parts, stearic acid 3-4 parts, HMPA 0.5-1 parts, sodium carboxymethylcellulose 1-2 parts, ten
Eight 2-3 parts of alcohol APEOs, ethylene glycol 3-4 parts, appropriate saturated sodium bicarbonate aqueous solution, appropriate deionized water.
2. the emamectin-benzoate mite killing suspending agent of the photoactivation synergy according to claims 1, it is special
Levy and be, 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；T-butyl methyl ether is added in organic phase, stirring makes it fully dissolve, room temperature
Lower addition benzoic acid, mixes reaction 5-6h, is slowly added dropwise 1/2 n-hexane, continues to mix reaction after completion of dropping
4-5h, filtering, filter cake is washed 2-3 times with remaining n-hexane, is vacuum dried, and obtains emamectin-benzoate；
（2）4 hydroxy coumarin, dichloromethane are added in reaction vessel, after mixing and stirring, phenylacetaldehyde and ring is added
Pentanone, continues mixing and stirring, adds nitromethane and triphenylphosphine, and reaction 8-10h is mixed at room temperature, filters,
Filter cake is added in ethyl acetate, mix 50-60min, using saturated sodium bicarbonate aqueous solution wash to solution substantially without
Color, vacuum distillation removes ethyl acetate, and recrystallization obtains modified furocoumarin compound；
（3）Nano-calcium carbonate is added in high-speed mixer, heat temperature raising stirring treats that temperature reaches 100-105 DEG C, and mixing is stirred
Mix 8-10min；By isopropyl three (dioctylphyrophosphoric acid acyloxy) titanate esters, step（1）Product, step（2）Product and
The solution of acetone configuration is sprayed on calcium carbonate while stirring, rises high-temperature to 120-130 DEG C, continues to mix 15-
20min, adds stearic acid, continues to stir mixing 18-20min；By material in 100-110 DEG C of discharge high-speed mixer, cool down,
It is standby
（4）By step（3）Product, HMPA, sodium carboxymethylcellulose be added to equivalent to step（3）Product
In the deionized water of 15-20 times of weight portion, ultrasonic disperse 30-40min adds polyoxyethylene octadecanol, ethylene glycol, with 800-
The rotating speed stirring 25-30min of 1000 turns/min, the emamectin-benzoate mite killing for obtaining photoactivation synergy suspends
Agent.
3. the emamectin-benzoate mite killing suspending agent of the photoactivation synergy according to claims 1,2, its
It is characterised by, the concentration of described phosphoric acid solution is 0.5-0.6mol/L.
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102475084A (en) * | 2010-11-25 | 2012-05-30 | 上海农乐生物制品股份有限公司 | Methylamino abamectin benzoate water dispersible granules and method for preparing same |
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2016
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102475084A (en) * | 2010-11-25 | 2012-05-30 | 上海农乐生物制品股份有限公司 | Methylamino abamectin benzoate water dispersible granules and method for preparing same |
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