CN109221133A - A kind of Pleocidin synergistic aqueous emulsion and preparation method thereof - Google Patents
A kind of Pleocidin synergistic aqueous emulsion and preparation method thereof Download PDFInfo
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- CN109221133A CN109221133A CN201811134797.9A CN201811134797A CN109221133A CN 109221133 A CN109221133 A CN 109221133A CN 201811134797 A CN201811134797 A CN 201811134797A CN 109221133 A CN109221133 A CN 109221133A
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- pleocidin
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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
- A01N43/22—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 rings with more than six members
-
- 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
Abstract
The present invention relates to technical field of pesticide preparations, specially a kind of Pleocidin synergistic aqueous emulsion and preparation method thereof, the aqueous emulsion is assembled by the raw material of following parts by weight: 1-15 parts of pleocidin, 10-25 parts of capsule casing material, 10-15 parts of organic solvent, 3-7 parts of emulsifier, 1-5 parts of synergist, 0.5-2.5 parts of wetting dispersing agent, 1-3 parts of surfactant, 1-3 parts of thickener, 2-4 parts of antifreeze, 3-5 parts of bleeding agent, 0.3-0.7 parts of defoaming agent, 50-70 parts of deionized water.Pleocidin synergistic aqueous emulsion of the present invention has good quick-acting, and high efficiency dispersion, efficacy stability is lasting, and storage life is long, and reduces the use of poisonous and harmful solvent, Environmental Safety.
Description
Technical field
The present invention relates to technical field of pesticide preparations, and in particular to a kind of Pleocidin synergistic aqueous emulsion and its preparation side
Method.
Background technique
Pleocidin is a kind of macrolides biological pesticide, has to pest and quickly tags and stomach poison function, but without interior
Suction effect, has stronger osmosis to blade, can kill subepidermal pest, and the residual period is longer, has one to some pests
Fixed ovicidal action, energy effectively preventing Lepidoptera, Diptera and Thysanoptera also can fine anti-smelting coleoptera and Orthopteras
In certain a large amount of feeding blades pest, but it is poor to the control efficiency of sucking pest and mite class.Pleocidin is to predation
Property natural enemy insect is safer, and with common insecticide no interactions resistance a few days ago.Composition containing pleocidin namely its
A possibility that compound preparation expands insecticidal spectrum and has synergistic effect, reduces resistance and raw mass-sending.Pleocidin is in environment
In it is degradable, therefore be particularly suited for the production of pollution-free vegetable, fruit, cereal.
Aqueous emulsion, which refers to, is dissolved in organic solvent acquired solution not soluble in water point for raw medicine liquid not soluble in water or raw medicine
It dissipates in one of water formulations of pesticide.Compared with other traditional formulations of pesticide especially missible oil product, due to water generation in aqueous emulsion
Having replaced reduces the dosage of organic solvent as decentralized medium for environment and the poisonous and hazardous organic solvent of people and animals, therefore has
There is environmental protection, without fire hazard, storage and convenient transportation, aqueous emulsion has become a weight of current formulations of pesticide development
Want direction.
The preparation of aqueous emulsion needs that the oil droplet in water phase is broken into micron-sized dispersity by the means of high shear,
Simultaneously by the addition of auxiliary agent is carried out chemistry package, drop low-surface-energy or using surface electric layer repulsive interaction make it is whole
A aqueous emulsion stable system, it is therefore desirable to select suitable auxiliary agent and suitable surfactant and solvent, can just prepare
Meet the aqueous emulsion of the indexs such as cold (heat) storage stability, dilution stability, pourability, viscosity.
By the retrieval to the prior art, in (the applying date: November 10 in 2009 of Chinese patent application 200910212246.4
Day) a kind of aqueous emulsion and preparation method thereof containing pleocidin is disclosed, which includes: A) kill more
Rhzomorph；B) avermectin perhaps emamectin-benzoate perhaps efficiently chlorine Flumethrin or lufenuron, Huo Zhegao
Imitate cypermethrin perhaps capillary perhaps chlorfluazuron perhaps diafenthiuron perhaps Diacloden or Fipronil.It is suitable by being added
When the auxiliary agents such as emulsifier, thickener, antifreezing agent, UV- protective agent, defoaming agent and surplus water, by certain processing work
Stable aqueous emulsion is made in skill.The technical solution of the invention be by two class active principles (pleocidin and another active material),
Emulsion dispersion is carried out after function additive, solvent and water mixing, to obtain multiple-effect preparation, but is occurred between these two types of active principles
Interference, causes the emulsion system stability to be formed poor, so that the validity of drug be caused to lose.
And in a kind of Chinese patent application patent 201010147003.X (applying date: the applying date: April 15 in 2010) pesticide
Aqueous emulsion and preparation method thereof.The effective component of the pesticide emulsion in water be penconazole, further include emulsifier, antifreeze, defoaming agent,
Solvent, thickener and water.The weight percentage of each component is respectively penconazole 1-30%, emulsifier 1-15%, antifreeze 1-
5%, defoaming agent 0-0.5%, solvent 1-45%, thickener 0.1-3%, water surplus.The aqueous emulsion the preparation method comprises the following steps: by penta bacterium
The a small amount of solvent of azoles and emulsifier dissolution, are uniformly mixing to obtain homogeneous oil phase；Then water, defoaming agent, antifreeze, thickener are stirred
Mixing is mixed, uniform water phase is formed, oil is added to water phase under room temperature and high-speed stirred or water phase is added to oily phase, is formed
Well dispersed aqueous emulsion, mixing speed are 200-3000 revs/min；Mixing time is 30-60 minutes；Use Laser particle-size distribution
Measure 2.00 microns of product cut size or less of instrument.But this medicament still remains preparation heat resistance deficiency and drug suspension
The poor problem of floating stability, this makes the validity period of medicament shorter, not can be carried out and saves for a long time.
Summary of the invention
Aiming at the problems existing in the prior art, the present invention provides a kind of Pleocidin synergistic aqueous emulsion and its preparation sides
Method, the aqueous emulsion have good quick-acting, and high efficiency dispersion, efficacy stability is lasting, and storage life is long, and reduce and toxic have
The use of evil solvent, Environmental Safety.
In order to achieve the above object, the present invention is achieved through the following technical solutions:
A kind of Pleocidin synergistic aqueous emulsion, the aqueous emulsion are assembled by the raw material of following parts by weight: more sterilizations
1-15 parts plain, 10-25 parts of capsule casing material, 10-15 parts of organic solvent, 3-7 parts of emulsifier, 1-5 parts of synergist, wetting dispersing agent
0.5-2.5 parts, 1-3 parts of surfactant, 1-3 parts of thickener, 2-4 parts of antifreeze, 3-5 parts of bleeding agent, defoaming agent 0.3-0.7
Part, 50-70 parts of deionized water；
Wherein, the pleocidin is solid content raw medicine, has the thermal stability higher than 100 DEG C, partial size is in 0.5-1.5
μm。
Preferably, the capsule casing material is beta-cyclodextrin and/or gamma-cyclodextrin.
Preferably, it is pungent to be selected from D- citric acid, ɑ-firpene, methyl abietate, N-Methyl pyrrolidone, N- for the organic solvent
It is one or more of in base pyrrolidones.
Preferably, the emulsifier is fatty alcohol polyoxyethylene ether, sorbitan monooleate, polyoxyethylene sorbitol
One or more of monolaurate.
Preferably, the synergist is palm oil methyloctanoic acid methyl esters and palm oil methyl methyl caprate is 3 in mass ratio:
1 mixture.
Preferably, the wetting dispersing agent is neopelex, sorbitol polyoxyethylene base ether, lignin sulfonic acid
Should, one or more of hydroxymethyl cellulose.
Preferably, in the surfactant anionic surfactant containing 65wt% and 35wt% nonionic table
Face activating agent；Anionic surfactant selects alpha-alkene sulfonate, lignosulfonates or triphenyl vinyl phenol polyoxyethylene
Ether phosphate；Nonionic surfactant selects Tween-80, alkyl glycosides, vinyl pyrrolidone or polyvinyl acetate
Ester.
Preferably, the thickener is xanthan gum, aluminum magnesium silicate or polyvinyl alcohol；The antifreeze is ethylene glycol, third
At least one of glycol, glycerine, diethylene glycol (DEG), urea.
Preferably, the bleeding agent is alkyl glycosides；The defoaming agent is poly- alkyl silicon ethylene oxide, in tributyl phosphate
One kind.
The present invention also provides the preparation methods of above-mentioned Pleocidin synergistic aqueous emulsion, comprising the following steps:
(1) pleocidin being weighed by mass fraction and being heated to molten condition, capsule casing material is added and stirs evenly, is then added
In emulsion dispersion equipment, adds emulsifier and carry out online-emulsification, obtain the average grain diameter of microcapsule particle at 0.5-1.5 μm；
(2) wetting dispersing agent is added in emulsion dispersion equipment, is formed and stablizes microcapsule suspension mother liquor；
(3) it according to mass fraction, adds organic solvents into Scattered Kettle, it is equal with the revolving speed dispersion of 450-550r/min
It is even, and microcapsule suspension mother liquor is added, uniform oily phase is formed after mixing；
(4) surfactant, thickener, antifreeze, bleeding agent, defoaming agent and deionized water are mixed, is added to reaction
In kettle, decentralized processing 6-8min, obtains water phase at a temperature of 50-60 DEG C；
(5) under the high shear machine effect that revolving speed is 2000-3000r/min, oil is mutually rapidly joined and shears shape in water phase
At lotion, high-speed stirred 15-20 minutes, bleeding agent and synergist are then added, and stir at low speed 5- in 800-1000r/min
8 minutes, obtain Pleocidin synergistic aqueous emulsion.
Major technique innovative point of the invention is:
(1) aqueous emulsion of the present invention extends pesticide validity period, intracapsular in this way has by the way that pleocidin is carried out coating processing
It imitates ingredient and effect partial is discharged by capsule casing material, due to the protection of softgel shell, effective component degradation speed slows down, pesticide
Lasting period is extended, simultaneously as the presence of softgel shell, the stability of pesticide is improved, so that drug can be with stable dispersion
In emulsion system, sedimentation, coalescence and the effect of other physical deteriorations will not occur, stability and the storage for improving pesticide are effective
Phase.
(2) it is 0.5-1.5 μm of microcapsule particle that partial size, which is made, in pleocidin by the present invention, in this way, can drug preferably
It is adsorbed on crop surface, so that better drug effect is played, meanwhile, the surface tension of pleocidin is reduced, so that pesticide is steady
It is qualitative to be improved.
(3) present invention has the palm oil methyloctanoic acid methyl esters and palm oil methyl capric acid first of synergistic effect by being added
Ester improves the control efficiency of pleocidin, reduces pleocidin using concentration and reduces costs.
(4) organic solvent in instant component and wetting dispersing agent can obtain oily phase for pleocidin is fully dispersed,
Emulsifier and surfactant generate synergistic effect, have fabulous synergistic effect, improve the stability of water and milk agent formulation.
Specific embodiment
Below with reference to embodiment, further description of the specific embodiments of the present invention, and following embodiment is only used for more
Technical solution of the present invention is clearly demonstrated, and not intended to limit the protection scope of the present invention.
Embodiment 1
The Pleocidin synergistic aqueous emulsion of the present embodiment, is assembled by the raw material of following parts by weight: pleocidin 1
Part, 10 parts of capsule casing material, 10 parts of organic solvent, 3 parts of emulsifier, 1 part of synergist, 0.5 part of wetting dispersing agent, surfactant 1
Part, 1 part of thickener, 2 parts of antifreeze, 3 parts of bleeding agent, 0.3 part of defoaming agent, 50 parts of deionized water；
Wherein, the pleocidin is solid content raw medicine, has the thermal stability higher than 100 DEG C, partial size is in 0.5-1.5
μm。
Wherein, the capsule casing material is beta-cyclodextrin and/or gamma-cyclodextrin.
Wherein, the organic solvent is selected from D- citric acid, ɑ-firpene, methyl abietate, N-Methyl pyrrolidone, N- octyl
It is one or more of in pyrrolidones.
Wherein, the emulsifier is fatty alcohol polyoxyethylene ether, sorbitan monooleate, polyoxyethylene sorbitol list
One or more of laurate.
Wherein, the synergist is palm oil methyloctanoic acid methyl esters and palm oil methyl methyl caprate is 3:1 in mass ratio
Mixture.
Wherein, the wetting dispersing agent is neopelex, sorbitol polyoxyethylene base ether, lignin sulfonic acid
Should, one or more of hydroxymethyl cellulose.
Wherein, in the surfactant anionic surfactant containing 65wt% and 35wt% non-ionic surface
Activating agent；Anionic surfactant selects alpha-alkene sulfonate, lignosulfonates or triphenyl vinyl phenol polyoxyethylene ether
Phosphate；Nonionic surfactant selects Tween-80, alkyl glycosides, vinyl pyrrolidone or polyvinyl acetate.
Wherein, the thickener is xanthan gum, aluminum magnesium silicate or polyvinyl alcohol；The antifreeze is ethylene glycol, the third two
At least one of alcohol, glycerine, diethylene glycol (DEG), urea.
Wherein, the bleeding agent is alkyl glycosides；The defoaming agent is poly- alkyl silicon ethylene oxide, in tributyl phosphate
It is a kind of.
The present invention also provides the preparation methods of above-mentioned Pleocidin synergistic aqueous emulsion, comprising the following steps:
(1) pleocidin being weighed by mass fraction and being heated to molten condition, capsule casing material is added and stirs evenly, is then added
In emulsion dispersion equipment, adds emulsifier and carry out online-emulsification, obtain the average grain diameter of microcapsule particle at 0.5-1.5 μm；
(2) wetting dispersing agent is added in emulsion dispersion equipment, is formed and stablizes microcapsule suspension mother liquor；
(3) it according to mass fraction, adds organic solvents into Scattered Kettle, is uniformly dispersed with the revolving speed of 450r/min, and
Microcapsule suspension mother liquor is added, forms uniform oily phase after mixing；
(4) surfactant, thickener, antifreeze, bleeding agent, defoaming agent and deionized water are mixed, is added to reaction
In kettle, decentralized processing 6min, obtains water phase at 50 °C；
(5) under the high shear machine effect that revolving speed is 2000r/min, oil is mutually rapidly joined into shearing in water phase and forms cream
Liquid high-speed stirred 15 minutes, then adds bleeding agent and synergist, and stir at low speed 5 minutes in 800r/min, obtains kill more
Rhzomorph synergistic aqueous emulsion.
Embodiment 2
The Pleocidin synergistic aqueous emulsion of the present embodiment, is assembled by the raw material of following parts by weight: pleocidin 15
Part, 25 parts of capsule casing material, 15 parts of organic solvent, 7 parts of emulsifier, 5 parts of synergist, 2.5 parts of wetting dispersing agent, surfactant 3
Part, 3 parts of thickener, 4 parts of antifreeze, 5 parts of bleeding agent, 0.7 part of defoaming agent, 70 parts of deionized water；
Wherein, the pleocidin is solid content raw medicine, has the thermal stability higher than 100 DEG C, partial size is in 0.5-1.5
μm。
Wherein, the capsule casing material is beta-cyclodextrin and/or gamma-cyclodextrin.
Wherein, the organic solvent is selected from D- citric acid, ɑ-firpene, methyl abietate, N-Methyl pyrrolidone, N- octyl
It is one or more of in pyrrolidones.
Wherein, the emulsifier is fatty alcohol polyoxyethylene ether, sorbitan monooleate, polyoxyethylene sorbitol list
One or more of laurate.
Wherein, the synergist is palm oil methyloctanoic acid methyl esters and palm oil methyl methyl caprate is 3:1 in mass ratio
Mixture.
Wherein, the wetting dispersing agent is neopelex, sorbitol polyoxyethylene base ether, lignin sulfonic acid
Should, one or more of hydroxymethyl cellulose.
Wherein, in the surfactant anionic surfactant containing 65wt% and 35wt% non-ionic surface
Activating agent；Anionic surfactant selects alpha-alkene sulfonate, lignosulfonates or triphenyl vinyl phenol polyoxyethylene ether
Phosphate；Nonionic surfactant selects Tween-80, alkyl glycosides, vinyl pyrrolidone or polyvinyl acetate.
Wherein, the thickener is xanthan gum, aluminum magnesium silicate or polyvinyl alcohol；The antifreeze is ethylene glycol, the third two
At least one of alcohol, glycerine, diethylene glycol (DEG), urea.
Wherein, the bleeding agent is alkyl glycosides；The defoaming agent is poly- alkyl silicon ethylene oxide, in tributyl phosphate
It is a kind of.
The present invention also provides the preparation methods of above-mentioned Pleocidin synergistic aqueous emulsion, comprising the following steps:
(1) pleocidin being weighed by mass fraction and being heated to molten condition, capsule casing material is added and stirs evenly, is then added
In emulsion dispersion equipment, adds emulsifier and carry out online-emulsification, obtain the average grain diameter of microcapsule particle at 0.5-1.5 μm；
(2) wetting dispersing agent is added in emulsion dispersion equipment, is formed and stablizes microcapsule suspension mother liquor；
(3) it according to mass fraction, adds organic solvents into Scattered Kettle, is uniformly dispersed with the revolving speed of 550r/min, and
Microcapsule suspension mother liquor is added, forms uniform oily phase after mixing；
(4) surfactant, thickener, antifreeze, bleeding agent, defoaming agent and deionized water are mixed, is added to reaction
In kettle, decentralized processing 8min at a temperature of 60 DEG C obtains water phase；
(5) under the high shear machine effect that revolving speed is 3000r/min, oil is mutually rapidly joined into shearing in water phase and forms cream
Liquid high-speed stirred 20 minutes, then adds bleeding agent and synergist, and stir at low speed 8 minutes in 1000r/min, obtains more
Bacteriocidin synergistic aqueous emulsion.
Embodiment 3
The Pleocidin synergistic aqueous emulsion of the present embodiment, is assembled by the raw material of following parts by weight: pleocidin 7.5
Part, 18 parts of capsule casing material, 13 parts of organic solvent, 5 parts of emulsifier, 3 parts of synergist, 1.5 parts of wetting dispersing agent, surfactant 2
Part, 2 parts of thickener, 3 parts of antifreeze, 4 parts of bleeding agent, 0.5 part of defoaming agent, 60 parts of deionized water；
Wherein, the pleocidin is solid content raw medicine, has the thermal stability higher than 100 DEG C, partial size is in 0.5-1.5
μm。
Wherein, the capsule casing material is beta-cyclodextrin and/or gamma-cyclodextrin.
Wherein, the organic solvent is selected from D- citric acid, ɑ-firpene, methyl abietate, N-Methyl pyrrolidone, N- octyl
It is one or more of in pyrrolidones.
Wherein, the emulsifier is fatty alcohol polyoxyethylene ether, sorbitan monooleate, polyoxyethylene sorbitol list
One or more of laurate.
Wherein, the synergist is palm oil methyloctanoic acid methyl esters and palm oil methyl methyl caprate is 3:1 in mass ratio
Mixture.
Wherein, the wetting dispersing agent is neopelex, sorbitol polyoxyethylene base ether, lignin sulfonic acid
Should, one or more of hydroxymethyl cellulose.
Wherein, in the surfactant anionic surfactant containing 65wt% and 35wt% non-ionic surface
Activating agent；Anionic surfactant selects alpha-alkene sulfonate, lignosulfonates or triphenyl vinyl phenol polyoxyethylene ether
Phosphate；Nonionic surfactant selects Tween-80, alkyl glycosides, vinyl pyrrolidone or polyvinyl acetate.
Wherein, the thickener is xanthan gum, aluminum magnesium silicate or polyvinyl alcohol；The antifreeze is ethylene glycol, the third two
At least one of alcohol, glycerine, diethylene glycol (DEG), urea.
Wherein, the bleeding agent is alkyl glycosides；The defoaming agent is poly- alkyl silicon ethylene oxide, in tributyl phosphate
It is a kind of.
The present invention also provides the preparation methods of above-mentioned Pleocidin synergistic aqueous emulsion, comprising the following steps:
(1) pleocidin being weighed by mass fraction and being heated to molten condition, capsule casing material is added and stirs evenly, is then added
In emulsion dispersion equipment, adds emulsifier and carry out online-emulsification, obtain the average grain diameter of microcapsule particle at 0.5-1.5 μm；
(2) wetting dispersing agent is added in emulsion dispersion equipment, is formed and stablizes microcapsule suspension mother liquor；
(3) it according to mass fraction, adds organic solvents into Scattered Kettle, is uniformly dispersed with the revolving speed of 500r/min, and
Microcapsule suspension mother liquor is added, forms uniform oily phase after mixing；
(4) surfactant, thickener, antifreeze, bleeding agent, defoaming agent and deionized water are mixed, is added to reaction
In kettle, decentralized processing 7min at a temperature of 55 DEG C obtains water phase；
(5) under the high shear machine effect that revolving speed is 2500r/min, oil is mutually rapidly joined into shearing in water phase and forms cream
Liquid high-speed stirred 18 minutes, then adds bleeding agent and synergist, and stir at low speed 6.5 minutes in 900r/min, obtains more
Bacteriocidin synergistic aqueous emulsion.
Embodiment 4
The Pleocidin synergistic aqueous emulsion of the present embodiment, is assembled by the raw material of following parts by weight: pleocidin 1-
15 parts, 10-25 parts of capsule casing material, 10-15 parts of organic solvent, 3-7 parts of emulsifier, 1-5 parts of synergist, wetting dispersing agent 0.5-
2.5 parts, 1-3 parts of surfactant, 1-3 parts of thickener, 2-4 parts of antifreeze, 3-5 parts of bleeding agent, 0.3-0.7 parts of defoaming agent, go
50-70 parts of ionized water；
Wherein, the pleocidin is solid content raw medicine, has the thermal stability higher than 100 DEG C, partial size is in 0.5-1.5
μm。
Wherein, the capsule casing material is beta-cyclodextrin and/or gamma-cyclodextrin.
Wherein, the organic solvent is selected from D- citric acid, ɑ-firpene, methyl abietate, N-Methyl pyrrolidone, N- octyl
It is one or more of in pyrrolidones.
Wherein, the emulsifier is fatty alcohol polyoxyethylene ether, sorbitan monooleate, polyoxyethylene sorbitol list
One or more of laurate.
Wherein, the synergist is palm oil methyloctanoic acid methyl esters and palm oil methyl methyl caprate is 3:1 in mass ratio
Mixture.
Wherein, the wetting dispersing agent is neopelex, sorbitol polyoxyethylene base ether, lignin sulfonic acid
Should, one or more of hydroxymethyl cellulose.
Wherein, in the surfactant anionic surfactant containing 65wt% and 35wt% non-ionic surface
Activating agent；Anionic surfactant selects alpha-alkene sulfonate, lignosulfonates or triphenyl vinyl phenol polyoxyethylene ether
Phosphate；Nonionic surfactant selects Tween-80, alkyl glycosides, vinyl pyrrolidone or polyvinyl acetate.
Wherein, the thickener is xanthan gum, aluminum magnesium silicate or polyvinyl alcohol；The antifreeze is ethylene glycol, the third two
At least one of alcohol, glycerine, diethylene glycol (DEG), urea.
Wherein, the bleeding agent is alkyl glycosides；The defoaming agent is poly- alkyl silicon ethylene oxide, in tributyl phosphate
It is a kind of.
The present invention also provides the preparation methods of above-mentioned Pleocidin synergistic aqueous emulsion, comprising the following steps:
(1) pleocidin being weighed by mass fraction and being heated to molten condition, capsule casing material is added and stirs evenly, is then added
In emulsion dispersion equipment, adds emulsifier and carry out online-emulsification, obtain the average grain diameter of microcapsule particle at 0.5-1.5 μm；
(2) wetting dispersing agent is added in emulsion dispersion equipment, is formed and stablizes microcapsule suspension mother liquor；
(3) it according to mass fraction, adds organic solvents into Scattered Kettle, it is equal with the revolving speed dispersion of 450-550r/min
It is even, and microcapsule suspension mother liquor is added, uniform oily phase is formed after mixing；
(4) surfactant, thickener, antifreeze, bleeding agent, defoaming agent and deionized water are mixed, is added to reaction
In kettle, decentralized processing 6-8min, obtains water phase at a temperature of 50-60 DEG C；
(5) under the high shear machine effect that revolving speed is 2000-3000r/min, oil is mutually rapidly joined and shears shape in water phase
At lotion, high-speed stirred 15-20 minutes, bleeding agent and synergist are then added, and stir at low speed 5- in 800-1000r/min
8 minutes, obtain Pleocidin synergistic aqueous emulsion.
Embodiment 5
The Pleocidin synergistic aqueous emulsion of the present embodiment, is assembled by the raw material of following parts by weight: pleocidin 1-
15 parts, 10-25 parts of capsule casing material, 10-15 parts of organic solvent, 3-7 parts of emulsifier, 1-5 parts of synergist, wetting dispersing agent 0.5-
2.5 parts, 1-3 parts of surfactant, 1-3 parts of thickener, 2-4 parts of antifreeze, 3-5 parts of bleeding agent, 0.3-0.7 parts of defoaming agent, go
50-70 parts of ionized water；
Wherein, the pleocidin is solid content raw medicine, has the thermal stability higher than 100 DEG C, partial size is in 0.5-1.5
μm。
Wherein, the capsule casing material is beta-cyclodextrin and/or gamma-cyclodextrin.
Wherein, the organic solvent is selected from D- citric acid, ɑ-firpene, methyl abietate, N-Methyl pyrrolidone, N- octyl
It is one or more of in pyrrolidones.
Wherein, the emulsifier is fatty alcohol polyoxyethylene ether, sorbitan monooleate, polyoxyethylene sorbitol list
One or more of laurate.
Wherein, the synergist is palm oil methyloctanoic acid methyl esters and palm oil methyl methyl caprate is 3:1 in mass ratio
Mixture.
Wherein, the wetting dispersing agent is neopelex, sorbitol polyoxyethylene base ether, lignin sulfonic acid
Should, one or more of hydroxymethyl cellulose.
Wherein, in the surfactant anionic surfactant containing 65wt% and 35wt% non-ionic surface
Activating agent；Anionic surfactant selects alpha-alkene sulfonate, lignosulfonates or triphenyl vinyl phenol polyoxyethylene ether
Phosphate；Nonionic surfactant selects Tween-80, alkyl glycosides, vinyl pyrrolidone or polyvinyl acetate.
Wherein, the thickener is xanthan gum, aluminum magnesium silicate or polyvinyl alcohol；The antifreeze is ethylene glycol, the third two
At least one of alcohol, glycerine, diethylene glycol (DEG), urea.
Wherein, the bleeding agent is alkyl glycosides；The defoaming agent is poly- alkyl silicon ethylene oxide, in tributyl phosphate
It is a kind of.
The present invention also provides the preparation methods of above-mentioned Pleocidin synergistic aqueous emulsion, comprising the following steps:
(1) pleocidin being weighed by mass fraction and being heated to molten condition, capsule casing material is added and stirs evenly, is then added
In emulsion dispersion equipment, adds emulsifier and carry out online-emulsification, obtain the average grain diameter of microcapsule particle at 0.5-1.5 μm；
(2) wetting dispersing agent is added in emulsion dispersion equipment, is formed and stablizes microcapsule suspension mother liquor；
(3) it according to mass fraction, adds organic solvents into Scattered Kettle, it is equal with the revolving speed dispersion of 450-550r/min
It is even, and microcapsule suspension mother liquor is added, uniform oily phase is formed after mixing；
(4) surfactant, thickener, antifreeze, bleeding agent, defoaming agent and deionized water are mixed, is added to reaction
In kettle, decentralized processing 6-8min, obtains water phase at a temperature of 50-60 DEG C；
(5) under the high shear machine effect that revolving speed is 2000-3000r/min, oil is mutually rapidly joined and shears shape in water phase
At lotion, high-speed stirred 15-20 minutes, bleeding agent and synergist are then added, and stir at low speed 5- in 800-1000r/min
8 minutes, obtain Pleocidin synergistic aqueous emulsion.
Comparative example 1
Capsule casing material is removed to and is cancelled the processing of pleocidin micro-capsule.
Comparative example 2
Other than saving synergist, other material contents and preparation step are consistent with embodiment 1.
Comparative example 3
In addition to pleocidin is changed to 0.5 especially, other material contents and preparation step are consistent with embodiment 1.
Comparative example 4
In addition to pleocidin is changed to 20 especially, other material contents and preparation step are consistent with embodiment 1.
Test example 1
The Pleocidin synergistic aqueous emulsion tested in the present embodiment and comparative example carries out hot storage, 0 ± 2 in 54 ± 2 DEG C of adjustings
DEG C and -15 ± 2 DEG C under the conditions of carry out low-temperature stability inspection, the results are shown in Table 1.
1 Pleocidin synergistic aqueous emulsion stability test result of table
It follows that stability can be improved by micro-capsule processing in pleocidin.
Test example 2
Prevent and treat paddy rice rice leaf roller worm field trial
The consistent rice of paddy rice rice leaf roller worm is chosen, medicament is directly diluted by spraying, 7 days, 15 days, 25 days after medicine with water
Leaf spot lesion area, investigation prevention effect are counted afterwards, and test result is shown in Table 2.
Table 2 prevents and treats paddy rice rice leaf roller worm test result
As shown in Table 2, the Pleocidin synergistic aqueous emulsion of the embodiment of the present invention imitates the prevention and treatment of paddy rice rice leaf roller worm
Fruit is better than the control efficiency of comparative example, surface by by micro- the progresss capsule processing of pleocidin, add synergist and by pleocidin
It is limited to the control efficiency that Pleocidin synergistic aqueous emulsion can be improved in given range.
In conclusion creativeness of the invention is mainly reflected in the following:
(1) aqueous emulsion of the present invention extends pesticide validity period, intracapsular in this way has by the way that pleocidin is carried out coating processing
It imitates ingredient and effect partial is discharged by capsule casing material, due to the protection of softgel shell, effective component degradation speed slows down, pesticide
Lasting period is extended, simultaneously as the presence of softgel shell, the stability of pesticide is improved, so that drug can be with stable dispersion
In emulsion system, sedimentation, coalescence and the effect of other physical deteriorations will not occur, stability and the storage for improving pesticide are effective
Phase.
(2) it is 0.5-1.5 μm of microcapsule particle that partial size, which is made, in pleocidin by the present invention, in this way, can drug preferably
It is adsorbed on crop surface, so that better drug effect is played, meanwhile, the surface tension of pleocidin is reduced, so that pesticide is steady
It is qualitative to be improved.
(3) present invention has the palm oil methyloctanoic acid methyl esters and palm oil methyl capric acid first of synergistic effect by being added
Ester improves the control efficiency of pleocidin, reduces pleocidin using concentration and reduces costs.
(4) organic solvent in instant component and wetting dispersing agent can obtain oily phase for pleocidin is fully dispersed,
Emulsifier and surfactant generate synergistic effect, have fabulous synergistic effect, improve the stability of water and milk agent formulation.
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, although referring to aforementioned reality
Applying example, invention is explained in detail, for those skilled in the art, still can be to aforementioned each implementation
Technical solution documented by example is modified or equivalent replacement of some of the technical features.It is all in essence of the invention
Within mind and principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of Pleocidin synergistic aqueous emulsion, which is characterized in that the aqueous emulsion assembled by the raw material of following parts by weight and
At: pleocidin 5%-40%, capsule casing material 5%-25%, organic solvent 3%-15%, emulsifier 0.5%-5%, synergist
1%-5%, wetting dispersing agent 0.2%-5%, 0-3 parts of surfactant, 1-3 parts of thickener, 2-4 parts of antifreeze, bleeding agent 3-5
Part, 0.3-0.7 parts of defoaming agent, 50-70 parts of deionized water；
Wherein, the pleocidin is solid content raw medicine, has the thermal stability higher than 100 DEG C, partial size is at 0.5-1.5 μm.
2. Pleocidin synergistic aqueous emulsion according to claim 1, which is characterized in that the capsule casing material is beta-cyclodextrin
And/or gamma-cyclodextrin.
3. Pleocidin synergistic aqueous emulsion according to claim 1, which is characterized in that the organic solvent is selected from D- lemon
It is one or more of in acid, ɑ-firpene, methyl abietate, N-Methyl pyrrolidone, n-octylpyrrolidone.
4. Pleocidin synergistic aqueous emulsion according to claim 1, which is characterized in that the emulsifier is fatty alcohol polyoxy
One or more of vinethene, sorbitan monooleate, polyoxyethylene sorbitan monolaurate.
5. Pleocidin synergistic aqueous emulsion according to claim 1, which is characterized in that the synergist is palm oil methyl
Methyl caprylate and palm oil methyl methyl caprate are the mixture of 3:1 in mass ratio.
6. Pleocidin synergistic aqueous emulsion according to claim 1, which is characterized in that the wetting dispersing agent is dodecane
Base benzene sulfonic acid sodium salt, sorbitol polyoxyethylene base ether, lignin sulfonic acid should, one or more of hydroxymethyl cellulose.
7. Pleocidin synergistic aqueous emulsion according to claim 1, which is characterized in that contain in the surfactant
The anionic surfactant of 65wt% and the nonionic surfactant of 35wt%；Anionic surfactant selects alpha-olefin
Sulfonate, lignosulfonates or triphenyl vinyl phenol polyoxyethylene ether phosphate；Nonionic surfactant selects poly- sorb
Ester -80, alkyl glycosides, vinyl pyrrolidone or polyvinyl acetate.
8. Pleocidin synergistic aqueous emulsion according to claim 1, which is characterized in that the thickener be xanthan gum,
Aluminum magnesium silicate or polyvinyl alcohol；The antifreeze is at least one of ethylene glycol, propylene glycol, glycerine, diethylene glycol (DEG), urea.
9. Pleocidin synergistic aqueous emulsion according to claim 1, which is characterized in that the bleeding agent is alkyl glycosides；
The defoaming agent is one of poly- alkyl silicon ethylene oxide, tributyl phosphate.
10. the preparation method of -9 described in any item Pleocidin synergistic aqueous emulsions according to claim 1, which is characterized in that packet
Include following steps:
(1) pleocidin being weighed by mass fraction and being heated to molten condition, capsule casing material is added and stirs evenly, emulsification is then added
In dispersing apparatus, adds emulsifier and carry out online-emulsification, obtain the average grain diameter of microcapsule particle at 0.5-1.5 μm；
(2) wetting dispersing agent is added in emulsion dispersion equipment, is formed and stablizes microcapsule suspension mother liquor；
(3) it according to mass fraction, adds organic solvents into Scattered Kettle, is uniformly dispersed with the revolving speed of 450-550r/min, and
Microcapsule suspension mother liquor is added, forms uniform oily phase after mixing；
(4) surfactant, thickener, antifreeze, bleeding agent, defoaming agent and deionized water are mixed, are added in reaction kettle,
Decentralized processing 6-8min, obtains water phase at a temperature of 50-60 DEG C；
(5) under the high shear machine effect that revolving speed is 2000-3000r/min, oil is mutually rapidly joined into shearing in water phase and forms cream
Liquid high-speed stirred 15-20 minutes, then adds bleeding agent and synergist, and stir at low speed 5-8 points in 800-1000r/min
Clock obtains Pleocidin synergistic aqueous emulsion.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110024790A (en) * | 2019-05-21 | 2019-07-19 | 山东圣鹏科技股份有限公司 | A kind of compounding and its application of the single dose containing multiple killing teichomycin |
| CN113016788A (en) * | 2021-03-24 | 2021-06-25 | 赤峰绿水青山生物科技有限公司 | Spinosad soluble agent and preparation method thereof |
Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1180476A (en) * | 1996-10-24 | 1998-05-06 | 冶金工业部长沙矿冶研究院 | Microcapsule water emulsion type composite herbicide |
| WO2001011963A1 (en) * | 1999-08-12 | 2001-02-22 | Eli Lilly And Company | Oral treatment of companion animals with ectoparasiticidal spinosyns |
| CN101669491A (en) * | 2009-09-25 | 2010-03-17 | 深圳诺普信农化股份有限公司 | Pesticide emulsion and preparation method thereof |
| CN101711525A (en) * | 2009-11-10 | 2010-05-26 | 深圳诺普信农化股份有限公司 | Water emulsion containing pleocidin and preparation method thereof |
| CN101790978A (en) * | 2009-12-02 | 2010-08-04 | 深圳诺普信农化股份有限公司 | Pesticide emulsion in water and preparation method thereof |
| CN102835397A (en) * | 2012-07-04 | 2012-12-26 | 河北威远生物化工股份有限公司 | Spinosad synergistic aqueous emulsion and preparation method thereof |
| CN102939970A (en) * | 2012-10-18 | 2013-02-27 | 上海沪联生物药业（夏邑）股份有限公司 | Microcapsule suspending agent containing spinosad and cyantraniliprole, and preparation method thereof |
| CN103518713A (en) * | 2013-10-12 | 2014-01-22 | 天津市华宇农药有限公司 | Synergist used in 5% avermectin emulsion in water |
| CN103918646A (en) * | 2014-04-22 | 2014-07-16 | 福建农林大学 | Synergystic pleocidin microsphere suspending agent and preparation method thereof |
-
2018
- 2018-09-28 CN CN201811134797.9A patent/CN109221133A/en active Pending
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1180476A (en) * | 1996-10-24 | 1998-05-06 | 冶金工业部长沙矿冶研究院 | Microcapsule water emulsion type composite herbicide |
| WO2001011963A1 (en) * | 1999-08-12 | 2001-02-22 | Eli Lilly And Company | Oral treatment of companion animals with ectoparasiticidal spinosyns |
| CN101669491A (en) * | 2009-09-25 | 2010-03-17 | 深圳诺普信农化股份有限公司 | Pesticide emulsion and preparation method thereof |
| CN101711525A (en) * | 2009-11-10 | 2010-05-26 | 深圳诺普信农化股份有限公司 | Water emulsion containing pleocidin and preparation method thereof |
| CN101790978A (en) * | 2009-12-02 | 2010-08-04 | 深圳诺普信农化股份有限公司 | Pesticide emulsion in water and preparation method thereof |
| CN102835397A (en) * | 2012-07-04 | 2012-12-26 | 河北威远生物化工股份有限公司 | Spinosad synergistic aqueous emulsion and preparation method thereof |
| CN102939970A (en) * | 2012-10-18 | 2013-02-27 | 上海沪联生物药业（夏邑）股份有限公司 | Microcapsule suspending agent containing spinosad and cyantraniliprole, and preparation method thereof |
| CN103518713A (en) * | 2013-10-12 | 2014-01-22 | 天津市华宇农药有限公司 | Synergist used in 5% avermectin emulsion in water |
| CN103918646A (en) * | 2014-04-22 | 2014-07-16 | 福建农林大学 | Synergystic pleocidin microsphere suspending agent and preparation method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110024790A (en) * | 2019-05-21 | 2019-07-19 | 山东圣鹏科技股份有限公司 | A kind of compounding and its application of the single dose containing multiple killing teichomycin |
| CN113016788A (en) * | 2021-03-24 | 2021-06-25 | 赤峰绿水青山生物科技有限公司 | Spinosad soluble agent and preparation method thereof |
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