CN107410295A - The Fluoxastrobin aqueous suspension agent of a kind of particle diameter less than 100 nanometers and preparation method thereof - Google Patents
The Fluoxastrobin aqueous suspension agent of a kind of particle diameter less than 100 nanometers and preparation method thereof Download PDFInfo
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- CN107410295A CN107410295A CN201710462207.4A CN201710462207A CN107410295A CN 107410295 A CN107410295 A CN 107410295A CN 201710462207 A CN201710462207 A CN 201710462207A CN 107410295 A CN107410295 A CN 107410295A
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- fluoxastrobin
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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
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/48—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with two nitrogen atoms as the only ring hetero atoms
- A01N43/54—1,3-Diazines; Hydrogenated 1,3-diazines
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- General Health & Medical Sciences (AREA)
- Dentistry (AREA)
- Plant Pathology (AREA)
- Engineering & Computer Science (AREA)
- Pest Control & Pesticides (AREA)
- Agronomy & Crop Science (AREA)
- Wood Science & Technology (AREA)
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Abstract
The Fluoxastrobin aqueous suspension agent of a kind of particle diameter less than 100 nanometers and preparation method thereof, belong to the production technical field of nano pesticide, Fluoxastrobin is dissolved in water ease of solubility organic solvent as organic phase, using water as aqueous phase, surfactant is added at least phase in aqueous phase or organic phase；Liquidated the method for blending by quick jet, and aqueous phase and organic phase turbulent closure scheme are collected with water or the water containing surfactant, and Fluoxastrobin aqueous suspension agent is made.Using aqueous suspension agent made of above method have particle diameter it is stable, it is scattered it is narrow, less than 100 nanometers, contribute to Drug absorbability resistance to wind and rain drop erosion, its infiltration and conduction to blade can be strengthened in blade face.And environmentally friendly, easy environment degradable, the characteristics of drug effect is high.
Description
Technical field
The invention belongs to the production technical field of nano pesticide, and in particular to the production skill of the agricultural chemicals suspension agent containing Fluoxastrobin
Art field.
Background technology
In pesticide field, often nano pesticide is defined as from the broadest scope of application：Particle diameter is less than 1 micron of particle.By
There is unique small size and high surface area effect in medicament nano particle, it shows excellent high-efficient characteristic.
Agricultural chemicals common dosage forms include：Pulvis, granula, fumicants, aqua, finish, suspending agent, emulsion etc..General pulvis, grain
Agent, more difficult absorbed of fumicants work, easily cause airborne dust, big for environment pollution.Many pesticide original medicines are relatively insoluble in water again simultaneously, difficult
In aqua is made.And be prepared into finish and then need to use a large amount of organic solvents, larger harm is caused to people and animals and environment.
Suspending agent is the highly important formulations of pesticide in modern, because it has preferable active compound water dispersible, less
Organic solvent usage amount and good wetability and exhibition put forth effort, meet modern and become to what less toxic efficiently direction was developed
Gesture.But current various suspending agents still generally existing problems with：1）Particle diameter is larger, easily floating or sedimentation, so as to cause layering or
Caking；2）Particle diameter distribution is wider, so as to cause Ostwald ripening；3）To prevent dispersion from occurring to reunite, it is necessary to add substantial amounts of
Surfactant.
The content of the invention
The present invention seeks to disclose, a kind of particle diameter is stable, disperses environmentally friendly Fluoxastrobin water narrow, less than 100 nanometers hangs
Floating agent.
The present invention is mainly made up of Fluoxastrobin, surfactant, water ease of solubility organic solvent and water.
The mass ratio of the Fluoxastrobin, surfactant and water ease of solubility organic solvent is 1: 0.2~10: 100~2000.
Above product of the present invention has the particle diameter stabilization of active compound composition Fluoxastrobin, disperses characteristics narrow, less than 100 nanometers,
Grain diameter is small and stablizes, and can remain no greater than 100 nm at least 3 weeks；Particle size distributions are narrow, and polydispersity coefficient PDI is less than
0.3.To people, animal and the safe and harmless noresidue of non-target organism, rat acute oral toxicity is more than 5000mg/kg, and percutaneous toxicity is big
In 4000mg/kg, it can rapidly be degraded by light and microorganism in soil, water and air, ultimately form carbon dioxide, to environment
Close friend, no destruction.
The present invention is another object is that propose the preparation method of above product.
Fluoxastrobin is dissolved in water ease of solubility organic solvent as organic phase, using water as aqueous phase, in aqueous phase or organic phase
In an at least phase in add surfactant；Liquidated the method for blending by quick jet, and aqueous phase and organic phase turbulent flow are mixed
Close, be collected with water or the water containing surfactant, Fluoxastrobin aqueous suspension agent is made.
Pesticide original medicine used in the present invention is the molten Fluoxastrobin of shipwreck, and Fluoxastrobin is that one kind can suppress almost all of true
The sprouting of Mycota germ spore and caused organic matter, also there is good inhibiting effect to Spores intrusion.Simultaneously as low
Toxogen medicine.
Using aqueous suspension agent made of above method have particle diameter it is stable, it is scattered it is narrow, less than 100 nanometers, contribute to medicine
Blade face is adsorbed in, resistance to wind and rain drop erosion, its infiltration and conduction to blade can be strengthened.And environmentally friendly, easy ring
The characteristics of border is degraded, drug effect is high.
Further, the mixing quality ratio of Fluoxastrobin of the present invention and surfactant, water ease of solubility organic solvent is 1
: 0.2~10: 100~2000.Needs can specifically be applied according to control of crop disease during use, can further be diluted with more water.
For the ratio of Fluoxastrobin and surfactant.Surfactant is very few to be less than 1: 0.2, the Fluoxastrobin nanometer of precipitation
Particle surface is too low by surfactant level of coverage, and nano particle can occur to reunite and size increases rapidly.And add excessive
Surfactant is more than 1: 10, and surfactant can not be completely dissolved in organic solvent before combination, can pre-formed surface work
Property agent micella particle, influence the service efficiency of surfactant during mixing, and particle diameter may be widened.Excessive surface in addition
The viscosity of two-phase, substantially reduces mixing turbulence effects when the addition of activating agent can greatly increase mixing.Therefore Fluoxastrobin is chosen
With the ratio 1: 0.2~10 of surfactant.
Determined for the ratio of Fluoxastrobin and water ease of solubility organic solvent by the solubility of Fluoxastrobin.Less than 1：100, phonetic bacterium
It can not be completely dissolved in organic solvent before ester mixing.And more than 1: 2000, it is most of after Fluoxastrobin organic solution mixes with water
Fluoxastrobin can not separate out from mixed liquor.Therefore 1: 100~2000 are chosen.
For the dosage of water, using very few water, after Fluoxastrobin organic solution mixes with water, most of Fluoxastrobin can not be from
Separated out in mixed liquor.Therefore it is at least about 10000 parts to choose water.Needs are specifically applied according to control of crop disease, can be used more
Water further dilutes.
The surfactant is the profit amphiphilic surfactant that HLB value is 8~16.With to people and animals and environment compared with
Safety nuisance free, easy environment degradable, it is environmentally friendly the characteristics of, improve the safety in utilization of finished product.Described surfactant
HLB value be 8 ~ 16, can preferably adsorb and stable water slurry is formed in dewatering medicament particle surface.
It is highly preferred that the profit amphiphilic surfactant be APG, profit amphipathic ethers, polyesters,
Polyamide-based, polysaccharide or protein-based block copolymer, amphipathic albumen, polyelectrolyte, tween, peregal, glycolipid, fat
In peptide, lipoprotein, aliphatic acid, phosphatide, betaine type compound at least any one.
Further, the profit amphiphilic surfactant is PLGA-PEG, Tween 80, APG APG.
The water ease of solubility organic solvent be ethanol, propyl alcohol, acetone, in dimethyl sulfoxide at least any one.This is a little molten
Agent is the 3rd class or the 4th class organic solvent, and organic solvent can be miscible with water, is allowed to intake without producing the per day of toxicity
Maximum dose（PDE）It is nuisanceless to environment more than 50 mg/days, the safety in utilization of finished product can be improved.
Brief description of the drawings
Fig. 1 is respectively using 30mL Fluoxastrobin nanometer aqueous suspension made from 3 ~ 30 μ L Tween 80s and 3 mg Fluoxastrobin active compounds
The time stability curve of agent particle diameter.
Fig. 2 is using 30 mL Fluoxastrobin nanometer waters made from 3 mg Fluoxastrobins active compounds and 0.6 ~ 3 mg PLGA-PEG difference
The time stability curve of suspending agent particle diameter.
Fig. 3 is to use 30 mL Fluoxastrobin nanometer aqueous suspension agents made from 3 mg Fluoxastrobins active compounds and 3 mg PLGA-PEG
Electron microscope.
Fig. 4 be respectively with quick jet liquidate mixing method and be added dropwise paddling process prepare contain 3 mg Fluoxastrobins active compounds and 3 mg
The time stability curve of PLGA-PEG 30mL Fluoxastrobin nanometer aqueous suspension agent particle diameters.
Fig. 5 be using 1.0 wt%APG as aqueous phase, with 3 mg Fluoxastrobin active compounds made from 30mL nanometer aqueous suspension agent grains
Footpath time stability curve.
Embodiment
In following example, the liquidate method and apparatus requirement of blending of quick jet is：
The quick jet blend method that liquidates is liquidated mixing for two strands and above fluid jet, each fluid streams Inlet Reynolds Number sum
More than 900, provide high jet for fluid and liquidate speed.Two miniature cavities volumes of used blender are less than 50 microlitres,
The fluid mixing holdup time is less than 150 milliseconds, and it is high-energy-density fast dissipation to make mixed process, and Efficient Conversion is nano particle
Surface energy, it is ensured that the nano particle diameter of preparation is less than 100nm polydispersity coefficients and is less than 0.3.
Example one：Prepare 30mL Fluoxastrobin nanometer aqueous suspension agents（The active compound of Fluoxastrobin containing 3mg, 3~30 μ L Tween 80s and 3.0mL
Ethanol）：
Take 3 μ L Tween 80s and 3mg Fluoxastrobin active compounds to be dissolved in 3.0mL ethanol, form organic phase.
3mL water is taken as aqueous phase.
Aqueous phase and organic phase are injected separately into two miniature cavities of blender, make two quick jets pair of miniature cavities
Punching, mix time-consuming about 5 seconds altogether.Mixed liquor is collected with the water containing 24mL, produces 30mL Fluoxastrobin nano suspension concentrates.
Using method of the same race, take 10,20,30 μ L Tween 80s to repeat above-mentioned experiment respectively, it is different to prepare Tween 80 content
Nano suspension concentrate, and dimension measurement is carried out to suspending agent with dynamic light scattering method, and track time stability.
As shown in figure 1, Tween 80 dosage is in 10~30 μ L（That is 3~10 times of Fluoxastrobin quality）When, suspending agent particle diameter compared with
Small, stability is good, and 50~100 nm can be maintained in one month, and the narrower PDI of particle diameter distribution is respectively less than 0.3.
Example two：Prepare 30mL Fluoxastrobin nanoscale aqueous suspension agents（The active compound of Fluoxastrobin containing 3mg, 0.6~3mg PLGA-PEG and
3.0 mL acetone）：
Take the amphipathic copolymer p LGA-PEG of 0.6 mg and 3 mg Fluoxastrobin active compounds to be dissolved in 3.0 mL acetone, form organic phase.
3mL water is taken as aqueous phase.
Aqueous phase and organic phase are injected separately into two miniature cavities of blender, make two quick jets pair of miniature cavities
Punching, mix time-consuming about 5 seconds altogether.With the container collection containing 24ml water, that is, obtain 30mL Fluoxastrobin suspending agents.
And with method of the same race, take 3mg PLGA-PEG to repeat above-mentioned experiment, the corresponding Fluoxastrobin nano suspension concentrates of 30mL are made.
Suspending agent is measured with dynamic light scattering method, initial mean diameter 83nm, PDI 0.29.And time stability is entered
Line trace is tested（As shown in Figure 2）.Granule-morphology size is have taken with ESEM（As shown in Figure 3）.
From Fig. 2,3：Use the stable Fluoxastrobins of 0.6~30mg PLGA-PEG（3mg）The nano suspending liquid being prepared
Particle diameter is small scattered narrow, and stability is good, and below 100nm can be maintained at least 3 weeks.
Example three：Be added dropwise paddling process and jet liquidate mixing method preparation compared with（30mL nanoscales aqueous suspension agent phonetic bacterium containing 3mg
Ester active compound, 3mg PLGA-PEG and 3.0mL propyl alcohol）：
Take 3mgPLGA-PEG and 3 mg Fluoxastrobin active compounds to be dissolved in 3.0mL propyl alcohol, form organic phase.
3mL water is taken as aqueous phase.
Aqueous phase and organic phase are injected separately into two miniature cavities of blender, make two quick jets pair of miniature cavities
Punching, mix time-consuming about 5 seconds altogether.With the container collection containing 24ml water, that is, obtain 30mL Fluoxastrobin suspending agents.
With identical proportioning, aqueous phase and organic phase are configured, 27mL water is slowly added dropwise into 3mL organic phases, is in rotating speed
Under the conditions of 900rpm, dripped off in 2 hours, obtain 30mL Fluoxastrobin suspension.
The test of time stability is carried out to suspending agent with dynamic light scattering.The mixing method as shown in figure 4, quick jet liquidates
The Fluoxastrobin suspension particle diameter of preparation is less than 100 nm, and is kept at least 3 weeks.And paddling process is added dropwise and prepares Fluoxastrobin suspension grain
Footpath is more than 200 nm, and 300nm is risen to after one week.Therefore the Fluoxastrobin suspension particle diameter for the mixing method preparation that liquidated by quick jet
It is smaller, stability is more preferable.
Respectively using above-mentioned jet liquidate aqueous suspension agent prepared by mixing method, aqueous suspension prepared by paddling process is added dropwise
Agent, certain commercially available situation of selling well import brand Fluoxastrobin aqueous suspension agent and water, first, second and third day to car li seed, cherry tomato,
Tomato surface is each uniformly to spray once, untill it can cover surface.Its antibacterial effect is listed in table one after two weeks, the results showed that passes through
Fluoxastrobin aqueous suspension of the antibacterial effect of Fluoxastrobin aqueous suspension agent prepared by the present invention prepared by far better than dropwise addition paddling process
Agent, and certain commercially available best seller brand Fluoxastrobin aqueous suspension agent.
Following table for respectively with quick jet liquidate Fluoxastrobin aqueous suspension agent prepared by mixing method, be added dropwise prepared by paddling process
Fluoxastrobin aqueous suspension agent, the antibacterial effect contrast table of certain commercially available brand Fluoxastrobin aqueous suspension agent and water.
Example four：Prepare 30mL Fluoxastrobin nanoscale aqueous suspension agents（Containing 30mgAPG, 3mg Fluoxastrobin active compound and 3mL dimethyl sulfoxides）：
Take 3mg Fluoxastrobin active compounds to be dissolved in 3mL dimethyl sulfoxides, form organic phase.
The 1.0 wt% APG APG aqueous solution is taken as 3mL aqueous phases.
Aqueous phase and organic phase are injected separately into two miniature cavities of blender, make two quick jets pair of miniature cavities
Punching, mix time-consuming about 5 seconds altogether.With the container collection equipped with the aqueous solution of the 24mL containing 1.0 wt% thickeners, that is, obtain Fluoxastrobin water
Suspension.
The test of time stability is carried out to suspension particle diameter with dynamic light scattering method, as a result as shown in Figure 5, it is seen that：With
For APG as surfactant, smaller initial particle is 43 nm.Slowly increase with time particle diameter, but at least one moon is still
Below 100nm can be maintained at.
Claims (8)
1. a kind of particle diameter is less than 100 nanometers of Fluoxastrobin aqueous suspension agent, it is characterised in that：Mainly by Fluoxastrobin, surfactant,
Water ease of solubility organic solvent and water composition.
2. Fluoxastrobin aqueous suspension agent according to claim 1, it is characterised in that：The Fluoxastrobin, surfactant and water
The mass ratio of ease of solubility organic solvent is 1: 0.2~10: 100~2000.
3. the preparation method of Fluoxastrobin aqueous suspension agent as claimed in claim 1, it is characterised in that：Fluoxastrobin is dissolved in water ease of solubility
Organic phase is used as in organic solvent, using water as aqueous phase, surfactant is added in an at least phase for aqueous phase or organic phase；It is logical
Too fast rapid fire stream is liquidated the method for blending, and by aqueous phase and organic phase turbulent closure scheme, the water with water or containing surfactant is carried out
Collect, Fluoxastrobin aqueous suspension agent is made.
4. preparation method according to claim 3, it is characterised in that：The Fluoxastrobin and surfactant, water ease of solubility
The mixing quality ratio of organic solvent is 1: 0.2~10: 100~2000.
5. preparation method according to claim 3, it is characterised in that：The surfactant is the oil that HLB value is 8~16
Water amphiphilic surfactant.
6. preparation method according to claim 3, it is characterised in that：The profit amphiphilic surfactant is alkyl sugar
Glycosides, profit amphipathic ethers, polyesters, polyamide-based, polysaccharide or protein-based block copolymer, amphipathic albumen, gather
It is at least any one in electrolyte, tween, peregal, glycolipid, lipopeptid, lipoprotein, aliphatic acid, phosphatide, betaine type compound
Kind.
7. preparation method according to claim 6, it is characterised in that：The profit amphiphilic surfactant is PLGA-
PEG, Tween 80, APG APG.
8. preparation method according to claim 3, it is characterised in that：The water ease of solubility organic solvent be ethanol, propyl alcohol,
In acetone, dimethyl sulfoxide at least any one.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710462207.4A CN107410295B (en) | 2017-06-19 | 2017-06-19 | Azoxystrobin water suspending agent with particle size less than 100 nanometers and preparation method thereof |
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| CN201710462207.4A CN107410295B (en) | 2017-06-19 | 2017-06-19 | Azoxystrobin water suspending agent with particle size less than 100 nanometers and preparation method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107996569A (en) * | 2017-12-12 | 2018-05-08 | 大庆华理生物技术有限公司 | Application of the biosurfactant lipopeptid in pesticide |
| CN108277186A (en) * | 2018-04-12 | 2018-07-13 | 扬州大学 | A kind of bacillus licheniformis and its application as pesticide surfactant |
| CN108353895A (en) * | 2018-01-30 | 2018-08-03 | 河北上瑞化工有限公司 | A kind of agricultural chemicals suspension agent using chitosan and azoxystrobin compound |
| WO2020136450A1 (en) * | 2018-12-28 | 2020-07-02 | 张子勇 | Miscible nano-sized pesticide suspension |
| CN115812722A (en) * | 2022-09-07 | 2023-03-21 | 深圳诺普信农化股份有限公司 | Nano pesticide water suspending agent and preparation method and application thereof |
| WO2024131333A1 (en) * | 2022-12-18 | 2024-06-27 | 张子勇 | Binary nanosuspension compounded with ester fungicide |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107996569A (en) * | 2017-12-12 | 2018-05-08 | 大庆华理生物技术有限公司 | Application of the biosurfactant lipopeptid in pesticide |
| CN108353895A (en) * | 2018-01-30 | 2018-08-03 | 河北上瑞化工有限公司 | A kind of agricultural chemicals suspension agent using chitosan and azoxystrobin compound |
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| WO2020136451A1 (en) * | 2018-12-28 | 2020-07-02 | 张子勇 | Method for preparing miscible nano-pesticide suspension |
| WO2020136450A1 (en) * | 2018-12-28 | 2020-07-02 | 张子勇 | Miscible nano-sized pesticide suspension |
| GB2587264A (en) * | 2018-12-28 | 2021-03-24 | Zhang Ziyong | Method for preparing miscible nano-pesticide suspension |
| GB2587264B (en) * | 2018-12-28 | 2022-11-09 | Zhang Ziyong | Method for preparing miscible nanosuspension |
| GB2585502B (en) * | 2018-12-28 | 2023-08-23 | Zhang Ziyong | Miscible nanosuspension |
| CN115812722A (en) * | 2022-09-07 | 2023-03-21 | 深圳诺普信农化股份有限公司 | Nano pesticide water suspending agent and preparation method and application thereof |
| WO2024131333A1 (en) * | 2022-12-18 | 2024-06-27 | 张子勇 | Binary nanosuspension compounded with ester fungicide |
| WO2024131337A1 (en) * | 2022-12-18 | 2024-06-27 | 张子勇 | Nano suspension comprising mancozeb, difenoconazole and prochloraz |
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