CN106797943A - A kind of emamectin-benzoate mite killing suspending agent with entrapping function and preparation method thereof - Google Patents
A kind of emamectin-benzoate mite killing suspending agent with entrapping function and preparation method thereof Download PDFInfo
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- CN106797943A CN106797943A CN201611202671.1A CN201611202671A CN106797943A CN 106797943 A CN106797943 A CN 106797943A CN 201611202671 A CN201611202671 A CN 201611202671A CN 106797943 A CN106797943 A CN 106797943A
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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
- 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
- A01N37/02—Saturated carboxylic acids or thio analogues thereof; Derivatives thereof
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- Pest Control & Pesticides (AREA)
- Agronomy & Crop Science (AREA)
- Wood Science & Technology (AREA)
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Abstract
A kind of emamectin-benzoate mite killing suspending agent with entrapping function, it is characterised in that it is prepared from by following raw material：Emamectin benzoate, methyl alcohol, phosphoric acid solution, toluene, isopropyl acetate, N, N double hydroxyethyls laurylamide, benzoic acid, n-hexane, cornstarch, carbohydrase, acetone, glycerin monostearate, 2 methylbutanoic acids are along 3 hexene esters, benzalkonium chloride, shitosan, acetic acid, lauroyl diethanolamine, atoleine, polyethyleneglycol diglycidylether, cetyl trimethylammonium bromide, calgon, methyl anyl alcohol, 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 with entrapping function
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 a kind of efficient and lasting emamectin benzoate benzene first with entrapping function
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 with entrapping function, 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, N, 2-3 parts of N- double hydroxyethyl laurylamides, benzoic acid 12-15 parts, n-hexane
180-200 parts, cornstarch 25-30 parts, carbohydrase 0.5-0.6 parts, acetone 150-180 parts, glycerin monostearate 3-4 parts,
4-5 parts of 2-Methyl Butyric Acid cis- 3- hexenes ester, benzalkonium chloride 3-4 parts, shitosan 18-20 parts, acetic acid 4-5 parts, lauroyl diethanol
Amine 2-3 parts, atoleine 80-100 parts, polyethyleneglycol diglycidylether 4-5 parts, cetyl trimethylammonium bromide 0.5-1
Part, calgon 2-3 parts, methyl anyl alcohol 3-4 parts, appropriate deionized water.
The described emamectin-benzoate mite killing suspending agent with entrapping function, 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；N, N- double hydroxyethyl laurylamides are added in organic phase, stirring makes it
Fully dissolving, adds benzoic acid at room temperature, mixes reaction 5-6h, is slowly added dropwise 1/2 n-hexane, continues after completion of dropping
Reaction 4-5h is mixed, filtering, filter cake is washed 2-3 times with remaining n-hexane, is vacuum dried, and obtains emamectin benzoate
Benzoate；
（2）Cornstarch is added in the deionized water equivalent to 4-5 times of cornstarch weight portion, after being well mixed, is placed in
In closed container, 105-115 DEG C of constant temperature stirs 18-20h, is cooled to room temperature, adds going equivalent to 1-2 times of corn weight portion
Ionized water, mixes 30-40min, and regulation system PH is 4-5, adds carbohydrase, 50-55 DEG C of constant temperature to stir 12-15h,
Dry, pulverize into the particle of 200-250 mesh；Add it in 2/3 acetone, ultrasonic disperse 40-50min is added single stearic
Acid glyceride, 45-50 DEG C of mixing 3-4h, is cooled to room temperature, adds step（1）Product, the cis- 3- hexenes of 2-Methyl Butyric Acid
Ester and benzalkonium chloride, continue to mix 2-3h, stand 10-12h, centrifugation, 50-60 DEG C of vacuum drying；
（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 lauroyl diethanolamine and atoleine configuration is added to, at 50-55 DEG C
25-30min is quickly stirred with the rotating speed constant temperature of 2200-2500 turns/min in water-bath, white " milky " liquid is formed, leads to nitrogen 20-
30min, adds the solution of polyethyleneglycol diglycidylether and the configuration of remaining acetone, and 65-70 DEG C is continued to stir 5-6h, is used
Deionized water is washed 2-3 times, and centrifugation dries 20-24h in 60-65 DEG C of vacuum drying chamber, obtains loading methylamino Avermectin
The chitosan sustained-release microsphere of plain benzoate；
（4）By step（3）Product, cetyl trimethylammonium bromide is added to equivalent to step（3）Products weight part 15-
In 20 times of deionized water, ultrasonic disperse 30-40min adds calgon, methyl anyl alcohol, with 800-1000 turns/min's
Rotating speed stirs 25-30min, obtains the emamectin-benzoate mite killing suspending agent with entrapping function.
The described emamectin-benzoate mite killing suspending agent with entrapping function, 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 present invention addition cis- 3- hexenes ester of 2-Methyl Butyric Acid, with methylamino Avermectin
Plain benzoate synergy, can lure acarid to lay eggs, and the hatching of ovum can be prevented again, or even ovum is killed, with " luring and destroy
It " effect, assign mite killing suspending agent entrapping function of the invention；The present invention wraps up AVM using shitosan, and uses
Polyethyleneglycol diglycidylether obtains sustained-release micro-spheres to chitosan crosslinked, can not only slow release medicine, extend medicament
Service life, can significantly reduce its resolution ratio in storage, and shitosan can promote medicament to be planted rapidly through Stoma of Leaves
Thing absorbs, and further increases miticidal effect；Mite killing suspending agent of the invention can efficiently lure acarid, effectively kill acarid, have
Excellent synergistic effect, reduces acaricidal field dosage, can effectively reduce residues of pesticides and the danger to beneficial organism
Evil, while reducing cost accounting and mitigating the pollution to environment.
Specific embodiment
The emamectin-benzoate mite killing suspending agent with entrapping function 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, N, 3 parts of N- double hydroxyethyls laurylamide, 15 parts of benzoic acid, 200 parts of n-hexane, 30 parts of cornstarch, carbohydrase
0.5 part, 180 parts of acetone, 4 parts of glycerin monostearate, 5 parts of the cis- 3- hexenes ester of 2-Methyl Butyric Acid, 4 parts of benzalkonium chloride, shitosan
20 parts, 5 parts of acetic acid, 3 parts of lauroyl diethanolamine, 100 parts of atoleine, 5 parts of polyethyleneglycol diglycidylether, cetyl
1 part of trimethylammonium bromide, 3 parts of calgon, 4 parts of methyl anyl alcohol, appropriate deionized water.
The emamectin-benzoate mite killing suspending agent with entrapping function 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；N, N- double hydroxyethyl laurylamides are added in organic phase, stirring makes it fully dissolve, room temperature
Lower addition benzoic acid, mixes reaction 6h, is slowly added dropwise 1/2 n-hexane, continues to mix reaction 5h after completion of dropping,
Filtering, filter cake is washed 3 times with remaining n-hexane, is vacuum dried, and obtains emamectin-benzoate；
（2）Cornstarch is added in the deionized water equivalent to 5 times of cornstarch weight portion, after being well mixed, is placed in close
Close in container, 115 DEG C of constant temperature stir 20h, are cooled to room temperature, add the deionized water equivalent to 2 times of corn weight portion, mixing
Stirring 40min, regulation system PH are 4-5, add carbohydrase, 55 DEG C of constant temperature to stir 15h, dry, pulverize into 250 purposes
Grain；Add it in 2/3 acetone, ultrasonic disperse 50min adds glycerin monostearate, 50 DEG C of mixing 4h, cooling
To room temperature, step is added（1）Product, the cis- 3- hexenes ester of 2-Methyl Butyric Acid and benzalkonium chloride, continue to mix 3h, stand
10-12h, centrifugation, 60 DEG C of vacuum drying；
（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, the solution of lauroyl diethanolamine and atoleine configuration is added to, in 55 DEG C of water-baths
25-30min is quickly stirred with the rotating speed constant temperature of 2500 turns/min, white " milky " liquid is formed, leads to nitrogen 30min, add poly- second
Hexanediol diglycidyl ether and the solution of remaining acetone configuration, 70 DEG C are continued to stir 6h, are washed with deionized 3 times, are centrifuged
Separate, 24h is dried in 65 DEG C of vacuum drying chambers, obtain loading the chitosan sustained-release microsphere of emamectin-benzoate；
（4）By step（3）Product, cetyl trimethylammonium bromide is added to equivalent to step（3）Products weight parts 20
In deionized water again, ultrasonic disperse 40min adds calgon, methyl anyl alcohol, is stirred with the rotating speed of 1000 turns/min
30min, obtains the emamectin-benzoate mite killing suspending agent with entrapping function.
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 | 81.6% | 90.1% |
| Heart-eating worm | 83.5% | 91.4% |
| Vegetable aphid | 83.5% | 90.4% |
| Planthopper | 81.4% | 89.7% |
| Acarid | 93.2% | 99.3% |
Claims (3)
1. a kind of emamectin-benzoate mite killing suspending agent with entrapping function, 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, N, 2-3 parts of N- double hydroxyethyl laurylamides, benzoic acid 12-15 parts, just oneself
Alkane 180-200 parts, cornstarch 25-30 parts, carbohydrase 0.5-0.6 parts, acetone 150-180 parts, glycerin monostearate 3-4
Part, 4-5 parts of 2-Methyl Butyric Acid cis- 3- hexenes ester, benzalkonium chloride 3-4 parts, shitosan 18-20 parts, acetic acid 4-5 parts, lauroyl two
Monoethanolamine 2-3 parts, atoleine 80-100 parts, polyethyleneglycol diglycidylether 4-5 parts, cetyl trimethylammonium bromide
0.5-1 parts, calgon 2-3 parts, methyl anyl alcohol 3-4 parts, appropriate deionized water.
2. the emamectin-benzoate mite killing suspending agent with entrapping function according to claims 1, 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；N, N- double hydroxyethyl laurylamides are added in organic phase, stirring makes it
Fully dissolving, adds benzoic acid at room temperature, mixes reaction 5-6h, is slowly added dropwise 1/2 n-hexane, continues after completion of dropping
Reaction 4-5h is mixed, filtering, filter cake is washed 2-3 times with remaining n-hexane, is vacuum dried, and obtains emamectin benzoate
Benzoate；
（2）Cornstarch is added in the deionized water equivalent to 4-5 times of cornstarch weight portion, after being well mixed, is placed in
In closed container, 105-115 DEG C of constant temperature stirs 18-20h, is cooled to room temperature, adds going equivalent to 1-2 times of corn weight portion
Ionized water, mixes 30-40min, and regulation system PH is 4-5, adds carbohydrase, 50-55 DEG C of constant temperature to stir 12-15h,
Dry, pulverize into the particle of 200-250 mesh；Add it in 2/3 acetone, ultrasonic disperse 40-50min is added single stearic
Acid glyceride, 45-50 DEG C of mixing 3-4h, is cooled to room temperature, adds step（1）Product, the cis- 3- hexenes of 2-Methyl Butyric Acid
Ester and benzalkonium chloride, continue to mix 2-3h, stand 10-12h, centrifugation, 50-60 DEG C of vacuum drying；
（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 lauroyl diethanolamine and atoleine configuration is added to, at 50-55 DEG C
25-30min is quickly stirred with the rotating speed constant temperature of 2200-2500 turns/min in water-bath, white " milky " liquid is formed, leads to nitrogen 20-
30min, adds the solution of polyethyleneglycol diglycidylether and the configuration of remaining acetone, and 65-70 DEG C is continued to stir 5-6h, is used
Deionized water is washed 2-3 times, and centrifugation dries 20-24h in 60-65 DEG C of vacuum drying chamber, obtains loading methylamino Avermectin
The chitosan sustained-release microsphere of plain benzoate；
（4）By step（3）Product, cetyl trimethylammonium bromide is added to equivalent to step（3）Products weight part 15-
In 20 times of deionized water, ultrasonic disperse 30-40min adds calgon, methyl anyl alcohol, with 800-1000 turns/min's
Rotating speed stirs 25-30min, obtains the emamectin-benzoate mite killing suspending agent with entrapping function.
3. the emamectin-benzoate mite killing suspending agent with entrapping function according to claims 1,2,
Characterized in that, the concentration of described phosphoric acid solution is 0.5-0.6mol/L.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611202671.1A CN106797943A (en) | 2016-12-23 | 2016-12-23 | A kind of emamectin-benzoate mite killing suspending agent with entrapping function and preparation method thereof |
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| CN201611202671.1A CN106797943A (en) | 2016-12-23 | 2016-12-23 | A kind of emamectin-benzoate mite killing suspending agent with entrapping function and preparation method thereof |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102823610A (en) * | 2012-09-14 | 2012-12-19 | 广东省昆虫研究所 | Anti-mite composition containing emamectin benzoate and hexythiazox |
| CN103497226A (en) * | 2013-10-11 | 2014-01-08 | 齐鲁晟华制药有限公司 | Refinement method of methylamino abamectin benzoate |
-
2016
- 2016-12-23 CN CN201611202671.1A patent/CN106797943A/en not_active Withdrawn
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102823610A (en) * | 2012-09-14 | 2012-12-19 | 广东省昆虫研究所 | Anti-mite composition containing emamectin benzoate and hexythiazox |
| CN103497226A (en) * | 2013-10-11 | 2014-01-08 | 齐鲁晟华制药有限公司 | Refinement method of methylamino abamectin benzoate |
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Application publication date: 20170606 |