CN106818790A - Good emamectin-benzoate mite killing suspending agent of a kind of being compatible with the environment property and preparation method thereof - Google Patents
Good emamectin-benzoate mite killing suspending agent of a kind of being compatible with the environment property and preparation method thereof Download PDFInfo
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- CN106818790A CN106818790A CN201611202560.0A CN201611202560A CN106818790A CN 106818790 A CN106818790 A CN 106818790A CN 201611202560 A CN201611202560 A CN 201611202560A CN 106818790 A CN106818790 A CN 106818790A
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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
- A01N25/10—Macromolecular compounds
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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 good emamectin-benzoate mite killing suspending agent of a kind of being compatible with the environment property, it is characterised in that it is prepared from by following raw material：Emamectin benzoate, methyl alcohol, phosphoric acid solution, toluene, isopropyl acetate, cetyl dimethicone, benzoic acid, n-hexane, Tea Polyphenols, ethyl acetate, sodium acid carbonate, caproyl chloride, soybean lecithin, HES, oleic acid, absolute ethyl alcohol, shitosan, acetic acid, stearoyl lactate, atoleine, hydroxyethyl methacrylate, capric acid triglyceride, Phenoxyethanol, Hostathion, 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 good emamectin benzoate benzene first of being compatible with the environment property
Hydrochlorate 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 good emamectin benzoate benzene of a kind of efficient and lasting being compatible with the environment property
Formates mite killing suspending agent and preparation method thereof.
To achieve these goals, the present invention is adopted the following technical scheme that：
The good emamectin-benzoate mite killing suspending agent of a kind of being compatible with the environment property, 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, cetyl dimethicone 2-3 parts, benzoic acid 12-15 parts, n-hexane
180-200 parts, Tea Polyphenols 2-3 parts, ethyl acetate 50-60 parts, sodium acid carbonate 1-2 parts, caproyl chloride 2-3 parts, soybean lecithin 5-6
Part, HES 18-20 parts, oleic acid 3-4 parts, absolute ethyl alcohol 40-50 parts, shitosan 18-20 parts, acetic acid 4-5 parts, stearoyl
Sodium lactate 2-3 parts, atoleine 80-100 parts, hydroxyethyl methacrylate 4-5 parts, 0.5-1 parts of capric acid triglyceride, benzene oxygen
Ethanol 2-3 parts, Hostathion 3-4 parts, appropriate deionized water.
The good emamectin-benzoate mite killing suspending agent of described being compatible with the environment property, it is characterised in that its
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；Cetyl dimethicone is added in organic phase, stirring makes its abundant
Dissolving, adds benzoic acid at room temperature, mixes reaction 5-6h, is slowly added dropwise 1/2 n-hexane, continues to mix after completion of dropping
Stirring reaction 4-5h, filtering, filter cake is washed 2-3 times with remaining n-hexane, is vacuum dried, and obtains emamectin benzoate benzene first
Hydrochlorate；
（2）Tea Polyphenols is added in ethyl acetate, mixing and stirring, rectifying to moisture is less than 2% in being transferred to rectifying column；
It is transferred in reactor, rises high-temperature to 65-75 DEG C, add sodium acid carbonate, after mixing 20-30min, is slowly added dropwise hexanoyl
Chlorine, continues to mix 8-10h after completion of dropping, is cooled to room temperature, and suction filtration is washed 2-3 times, dried；By dried product,
In being added to absolute ethyl alcohol together with soybean lecithin, HES, oleic acid, add equivalent to equivalent to soybean lecithin weight portion
5-6 times of deionized water, is put into 60-65 DEG C of water-bath dissolving in constant-temperature heating magnetic stirring apparatus, adds step（1）Product, 75-
80 DEG C are continued to mix 10-12h, stand 20-24h, and filtering is dried；
（3）By step（2）Product, shitosan is added to acetic acid and matches somebody with somebody equivalent to the deionized water of 30-35 times of acetic acid weight portion
In the solution put, after mixing and stirring, the solution of stearoyl lactate and atoleine configuration is added to, in 50-55 DEG C of water
25-30min is quickly stirred with the rotating speed constant temperature of 2200-2500 turns/min in bath, white " milky " liquid is formed, leads to nitrogen 20-
30min, adds hydroxyethyl methacrylate, and 65-70 DEG C is continued to stir 5-6h, is washed with deionized 2-3 times, centrifugation point
From, 20-24h is dried in 60-65 DEG C of vacuum drying chamber, the chitosan sustained-release for obtaining loading emamectin-benzoate is micro-
Ball；
（4）By step（3）Product, capric acid triglyceride is added to equivalent to step（3）Products weight part 15-20 times
In deionized water, ultrasonic disperse 30-40min adds Phenoxyethanol, Hostathion, and 25- is stirred with the rotating speed of 800-1000 turns/min
30min, obtains the good emamectin-benzoate mite killing suspending agent of being compatible with the environment property.
The good emamectin-benzoate mite killing suspending agent of described being compatible with the environment property, it is characterised in that institute
The concentration of the phosphoric acid solution stated 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, and will not produce resistance；Methylamino
Abamectin benzoate belongs to biogenic pesticide, with its unique mechanism of action, be difficult to remain, can be biodegradable, safety,
Environmentally friendly the advantages of, meet the nuisanceless fruits and vegetables of development, the requirement of pollution-free food；Present invention addition Tea Polyphenols, with methylamino Avermectin
Plain benzoate synergy, can not only kill insect, evil mite, worm's ovum, and can kill pathogen, increase the present invention outstanding
Floating agent miticidal effect；Mite killing effective ingredient of the present invention belongs to biological source medicament and medicine based on herbs, and being compatible with the environment property is good, can quilt
Biodegradation, it is safe and efficient；The present invention wraps up AVM using shitosan, and using hydroxyethyl methacrylate to shitosan
Crosslinking, obtains sustained-release micro-spheres, can not only slow release medicine, extend the service life of medicament, it can be significantly reduced and store
Middle resolution ratio is deposited, and shitosan can promote medicament to be absorbed by plants rapidly through Stoma of Leaves, further increase miticidal effect；This
The mite killing suspending agent of invention can efficiently lure acarid, effectively kill acarid, with excellent synergistic effect, reduce acaricidal
Field dosage, can effectively reduce residues of pesticides and the harm to beneficial organism, while reducing cost accounting and mitigating to ring
The pollution in border.
Specific embodiment
The good emamectin-benzoate mite killing suspending agent of the being compatible with the environment property of the present embodiment, it by weighing as follows
The raw material for measuring part is prepared from：8 parts of emamectin benzoate, 150 parts of methyl alcohol, 40 parts of phosphoric acid solution, 250 parts of toluene, acetic acid are different
70 parts of propyl ester, 3 parts of cetyl dimethicone, 15 parts of benzoic acid, 200 parts of n-hexane, 3 parts of Tea Polyphenols, ethyl acetate 60
Part, 2 parts of sodium acid carbonate, 3 parts of caproyl chloride, 6 parts of soybean lecithin, 20 parts of HES, 4 parts of oleic acid, 50 parts of absolute ethyl alcohol, shell gather
20 parts of sugar, 5 parts of acetic acid, 3 parts of stearoyl lactate, 100 parts of atoleine, 5 parts of hydroxyethyl methacrylate, the acid glycerol of capric acid three
1 part of ester, 3 parts of Phenoxyethanol, 3 parts of Hostathion, appropriate deionized water.
The good emamectin-benzoate mite killing suspending agent of the being compatible with the environment property of the present embodiment, it by walking as follows
Suddenly 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；Cetyl dimethicone is added in organic phase, stirring makes it fully dissolve, added at room temperature
Enter benzoic acid, mix reaction 6h, be slowly added dropwise 1/2 n-hexane, continue to mix reaction 5h, mistake after completion of dropping
Filter, filter cake is washed 3 times with remaining n-hexane, is vacuum dried, and obtains emamectin-benzoate；
（2））Tea Polyphenols is added in ethyl acetate, mixing and stirring, rectifying to moisture is less than 2% in being transferred to rectifying column；
It is transferred in reactor, rises high-temperature to 75 DEG C, add sodium acid carbonate, after mixing 30min, be slowly added dropwise caproyl chloride, drips
To add continue after finishing and mix 10h, be cooled to room temperature, suction filtration is washed 3 times, dried；By dried product, with soybean phosphorus
Fat, HES, oleic acid are added in absolute ethyl alcohol together, are added equivalent to going equivalent to 6 times of soybean lecithin weight portion
Ionized water, is put into 65 DEG C of water-bath dissolvings in constant-temperature heating magnetic stirring apparatus, adds step（1）Product, 80 DEG C continue mixing stir
12h is mixed, 24h is stood, filtering is dried；
（3）By step（2）Product, shitosan is added to acetic acid and configures equivalent to the deionized water of 35 times of acetic acid weight portion
In solution, after mixing and stirring, be added to stearoyl lactate and atoleine configuration solution, in 55 DEG C of water-baths with
The rotating speed constant temperature of 2500 turns/min quickly stirs 30min, forms white " milky " liquid, leads to nitrogen 30min, adds methacrylic acid
Hydroxyl ethyl ester, 70 DEG C are continued to stir 6h, are washed with deionized 3 times, centrifugation, and 24h is dried in 65 DEG C of vacuum drying chambers, are obtained
Load the chitosan sustained-release microsphere of emamectin-benzoate；
（4）By step（3）Product, capric acid triglyceride is added to equivalent to step（3）Products weight parts 20 times go
In ionized water, ultrasonic disperse 40min adds Phenoxyethanol, Hostathion, and 30min is stirred with the rotating speed of 1000 turns/min, obtain with
The good emamectin-benzoate mite killing suspending agent of Environmental compatibility.
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 | 80.3% | 89.9% |
| Heart-eating worm | 81.7% | 91.1% |
| Vegetable aphid | 82.5% | 93.4% |
| Planthopper | 80.4% | 90.7% |
| Acarid | 91.4% | 98.9% |
Claims (3)
1. the good emamectin-benzoate mite killing suspending agent of a kind of being compatible with the environment property, it is characterised in that it is by such as
The raw material of lower 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, cetyl dimethicone 2-3 parts, benzoic acid 12-15 parts, n-hexane
180-200 parts, Tea Polyphenols 2-3 parts, ethyl acetate 50-60 parts, sodium acid carbonate 1-2 parts, caproyl chloride 2-3 parts, soybean lecithin 5-6
Part, HES 18-20 parts, oleic acid 3-4 parts, absolute ethyl alcohol 40-50 parts, shitosan 18-20 parts, acetic acid 4-5 parts, stearoyl
Sodium lactate 2-3 parts, atoleine 80-100 parts, hydroxyethyl methacrylate 4-5 parts, 0.5-1 parts of capric acid triglyceride, benzene oxygen
Ethanol 2-3 parts, Hostathion 3-4 parts, appropriate deionized water.
2. the good emamectin-benzoate mite killing suspending agent of being compatible with the environment property according to claims 1,
Characterized in that, 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；Cetyl dimethicone is added in organic phase, stirring makes its abundant
Dissolving, adds benzoic acid at room temperature, mixes reaction 5-6h, is slowly added dropwise 1/2 n-hexane, continues to mix after completion of dropping
Stirring reaction 4-5h, filtering, filter cake is washed 2-3 times with remaining n-hexane, is vacuum dried, and obtains emamectin benzoate benzene first
Hydrochlorate；
（2））Tea Polyphenols is added in ethyl acetate, mixing and stirring, rectifying to moisture is less than 2% in being transferred to rectifying column；
It is transferred in reactor, rises high-temperature to 65-75 DEG C, add sodium acid carbonate, after mixing 20-30min, is slowly added dropwise hexanoyl
Chlorine, continues to mix 8-10h after completion of dropping, is cooled to room temperature, and suction filtration is washed 2-3 times, dried；By dried product,
In being added to absolute ethyl alcohol together with soybean lecithin, HES, oleic acid, add equivalent to equivalent to soybean lecithin weight portion
5-6 times of deionized water, is put into 60-65 DEG C of water-bath dissolving in constant-temperature heating magnetic stirring apparatus, adds step（1）Product, 75-
80 DEG C are continued to mix 10-12h, stand 20-24h, and filtering is dried；
（3）By step（2）Product, shitosan is added to acetic acid and matches somebody with somebody equivalent to the deionized water of 30-35 times of acetic acid weight portion
In the solution put, after mixing and stirring, the solution of stearoyl lactate and atoleine configuration is added to, in 50-55 DEG C of water
25-30min is quickly stirred with the rotating speed constant temperature of 2200-2500 turns/min in bath, white " milky " liquid is formed, leads to nitrogen 20-
30min, adds hydroxyethyl methacrylate, and 65-70 DEG C is continued to stir 5-6h, is washed with deionized 2-3 times, centrifugation point
From, 20-24h is dried in 60-65 DEG C of vacuum drying chamber, the chitosan sustained-release for obtaining loading emamectin-benzoate is micro-
Ball；
（4）By step（3）Product, capric acid triglyceride is added to equivalent to step（3）Products weight part 15-20 times
In deionized water, ultrasonic disperse 30-40min adds Phenoxyethanol, Hostathion, and 25- is stirred with the rotating speed of 800-1000 turns/min
30min, obtains the good emamectin-benzoate mite killing suspending agent of being compatible with the environment property.
3. the good emamectin-benzoate mite killing of being compatible with the environment property according to claims 1,2 suspends
Agent, it is characterised in that the concentration of described phosphoric acid solution is 0.5-0.6mol/L.
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| CN201611202560.0A CN106818790A (en) | 2016-12-23 | 2016-12-23 | Good emamectin-benzoate mite killing suspending agent of a kind of being compatible with the environment property and preparation method thereof |
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101622987A (en) * | 2008-10-24 | 2010-01-13 | 江西正邦化工有限公司 | Emamectin benzoate microcapsule suspending agent and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101622987A (en) * | 2008-10-24 | 2010-01-13 | 江西正邦化工有限公司 | Emamectin benzoate microcapsule suspending agent and preparation method thereof |
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Application publication date: 20170613 |
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