CN107136057A - A kind of highly effective and safe pyrethrin nanometer aqueous emulsion and preparation method thereof - Google Patents
A kind of highly effective and safe pyrethrin nanometer aqueous emulsion and preparation method thereof Download PDFInfo
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- CN107136057A CN107136057A CN201710525957.1A CN201710525957A CN107136057A CN 107136057 A CN107136057 A CN 107136057A CN 201710525957 A CN201710525957 A CN 201710525957A CN 107136057 A CN107136057 A CN 107136057A
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- pyrethrin
- aqueous emulsion
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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
-
- 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
- A01N65/00—Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof
- A01N65/08—Magnoliopsida [dicotyledons]
- A01N65/12—Asteraceae or Compositae [Aster or Sunflower family], e.g. daisy, pyrethrum, artichoke, lettuce, sunflower, wormwood or tarragon
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- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
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- Plant Pathology (AREA)
- Environmental Sciences (AREA)
- Agronomy & Crop Science (AREA)
- Natural Medicines & Medicinal Plants (AREA)
- Zoology (AREA)
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- Microbiology (AREA)
- Biotechnology (AREA)
- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Pest Control & Pesticides (AREA)
- Toxicology (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
A kind of highly effective and safe pyrethrin nanometer aqueous emulsion and preparation method thereof, belong to nano-pesticide formulation production technical field, pyrethrosin primary medicine and emulsifying agent are dissolved in acetone and are used as oil phase, it regard water as aqueous phase, by aqueous phase and oil phase in microcavity body high speed jet mixing, 200 below nm pyrethrin water emulsion insecticide is obtained.Active component is that natural plant extracts do not develop immunity to drugs, and contained all compositions are almost non-toxic to people and animals, the degradable, noresidue in external environment, is a kind of efficient pesticides to environment, agricultural product, people and animals with high security.
Description
Technical field
The invention belongs to nano-pesticide formulation production technical field, and in particular to pyrethrin nanometer aqueous emulsion formula and
Production method.
Background technology
With the development and the expansion of agriculture scale of society, the demand to agricultural chemicals is growing day by day, some efficient, high residues
Chemical pesticide preparation rapid rising.But with the raising of people's environmental consciousness in recent years and the progress of technology, agricultural chemicals starts to follow peace
Entirely, principle economic, effective, easy to use, develops to nontoxic, environmentally friendly, low-residual direction.Green and environment-friendly pesticide turns at present to be opened
The focus of hair.
Aqueous emulsion is highly important a kind of formulations of pesticide in modern, because its have preferable active compound water dispersible,
Less organic solvent usage amount and good wetability and exhibition are puted forth effort, and meet what modern developed to the efficient direction of low toxicity
Trend.But the following defect of current aqueous emulsion still generally existing：1）Size droplet diameter is larger, easily floating or sedimentation, so as to cause layering；
2）Particle diameter distribution is wider so as to cause Ostwald ripening；3）To prevent dispersion from occurring aggregation layering, it is necessary to add substantial amounts of breast
Agent.In view of the foregoing, the space that the drug effect of pesticide emulsion in water still improves a lot, the mesh for applying synergy is significantly subtracted to realize
's.
The content of the invention
Present invention aims at propose that a kind of drop size is stable, monodispersity is good, safe and efficient pyrethrin nanometer
Aqueous emulsion.
The highly effective and safe pyrethrin nanometer aqueous emulsion of the present invention is made up of pyrethrin, emulsifying agent, acetone and water.
The present invention also proposes the preparation method of above pyrethrin nanometer aqueous emulsion：Pyrethrosin primary medicine and emulsifying agent is molten
As oil phase in acetone, using water as aqueous phase, by aqueous phase and oil phase in microcavity body high speed jet mixing, pyrethrin is made
Nanometer aqueous emulsion.
The present invention is by easy environment degradable, non-harmful pyrethrosin primary medicine and emulsifying agent PLGA-b- PEG is dissolved in non-harmful
In organic solvent-acetone, with water in microcavity body high speed jet mixing, 200 below nm are obtained after jet mixing in microcavity body
The stable pyrethrin water emulsion insecticide of drop size, emulsion droplet is small and stablize, can keep at least one moon, particle chi
Very little scattered narrow, polydispersity coefficient PDI is less than 0.3.Needs can specifically be applied according to control of crop disease when using, more water can be used
Further dilution.
It is of the invention preferential from acetone as the readily soluble organic solvent of water in present invention process, can dissolve pyrethrin and
PLGA-b- PEG, and can be miscible with water.According to the toxicity of acetone, it is the 3rd or the 4th class solvent, and daily intake is not more than
It is at least 50mg/ days, nuisanceless to environment.
Further, the volume ratio of the pyrethrin, emulsifying agent, water ease of solubility organic solvent, water for 1: 0.018~
0.2∶9∶10。
For pyrethrosin primary medicine and emulsifying agent PLGA-b- PEG ratio.Emulsifying agent is very few to be less than 1: 0.018, Dalmatian chrysanthemum
It is too low that plain nano-liquid droplet surface is emulsified agent level of coverage, and nano-liquid droplet can occur to reunite and size increases rapidly.And added
Multi-surface activating agent is more than 1: 0.2, and emulsifying agent can not be completely dissolved in organic solvent before combination, the pre-formed emulsifying agent of meeting
Micella particle, the service efficiency of emulsifying agent during influence mixing, and size droplet diameter may be widened.Therefore pyrethrosin primary medicine is chosen
With emulsifying agent（Amphipathic nature block polymer PLGA-b-PEG）Ratio be 1: 0.018~0.2.
Ratio for pyrethrin and acetone is determined by the solubility of pyrethrin.When being significantly smaller than 1: 9, pyrethrin
It can not be completely dissolved in acetone before mixing.And when being far longer than 1: 9, it is most of after pyrethrin acetone soln is mixed with water
Pyrethrin can not be separated out from mixed liquor.Therefore 1: 9 is chosen.
For the consumption of water, it should equal to the pyrethrin and acetone sum of liquid, to reach that two-phase can be mixed in equal volume
Fully.Therefore it is 10 parts to choose water.Mix and needs are specifically applied according to desinsection, can further have been diluted with more water.
The Reynolds number sum of each jet inlet is more than 2200 in described microcavity body, it is ensured that energy is sufficiently high to reach mixing
Abundant turbulent flow, while mixing chamber volume is less than 0.1 mL, it is ensured that energy concentrates dissipation, Efficient Conversion to be droplet surface energy, reaches
To prepared size droplet diameter is small, narrowly distributing.
Pyrethrin nanometer aqueous emulsion of the present invention can be used as hygienic daily class, pets, plant protection insecticides.This is received
The features such as rice milk liquid has size droplet diameter small and narrow ditribution, stability are good, drug effect is high, active component be natural plant extracts not
Develop immunity to drugs, contained all compositions are almost non-toxic to people and animals, the degradable, noresidue in external environment, be a kind of to ring
Border, agricultural product, people and animals have the efficient spectrum insecticide of high security.
Pyrethrosin primary medicine used in the present invention is a kind of oily hydrophobic mixture for being isolated from pyrethrum flowers.Can conduct
Natural broad spectrum pesticide, and drug resistance will not be produced.Water and carbon dioxide can be resolved under light conditions, with its preparation
Insecticide uses rear drug residue free.Pyrethrin is extremely low to people and animals' toxicity, has no side effect.Tests prove that it is to warm-blooded animal
Toxicity only with salt（LD50,3000mg/kg）Quite, rat acute LD50 is 2330 mg/kg（It is female）And 3160mg/
kg（It is male）.
Emulsifying agent of the present invention is the amphipathic nature block polymer PLGA- that can be medical and edible of FDA certificationsb-PEG。
It has the advantage of nontoxic, nuisanceless, easy environment degradable, can further ensure the environmentally friendly property for the emulsifying agent being made.
Brief description of the drawings
Fig. 1 is to use PLGA-b- PEG is the grain size distribution of nanoemulsions made from emulsifying agent.
Fig. 2 is to use different amounts of PLGA-b- PEG is bent for the time stability of nanometer water emulsion particle diameter made from emulsifying agent
Line chart.
Fig. 3 is stable using the time that paddling process and nanometer water emulsion particle diameter made from high-speed jet mixing method is added dropwise respectively
Linearity curve figure.
Embodiment
In following example, in the method and apparatus requirement of microcavity body high speed jet mixing：
Method is：First oil phase and aqueous phase are injected separately into by two diameter 0.5mm entrances in the cavity that volume is 30 μ L and mixed,
Oil phase and aqueous phase are liquidated with 1.5m/s injection flow velocity respectively, and the Inlet Reynolds Number sum of gained two is about 2700.
These hybrid parameters can ensure that the quick high-energy-density of mixing dissipates there is provided the high surface energy of emulsion droplet, make shape
Into nanoemulsions there is small particle diameter, narrow ditribution, high stability the characteristics of.
Example one：Prepare 10 mL pyrethrins nanometer aqueous emulsions（Contain 4.5,9,18,36,45 or 100 mg PLGA- respectivelyb-
PEG and 0.5 mL pyrethrosin primary medicines）.
Take 45 mg PLGA-b- PEG and 0.5 mL pyrethrosin primary medicines are dissolved in 4.5 mL acetone, form organic phase.
5 mL water are taken as aqueous phase.
Aqueous phase and organic phase are injected in the microcavity of high-speed jet mixing apparatus by two entrances respectively, blended, mixing
Liquid is flowed out from cavity outlet, and pyrethrin nanoemulsions are obtained with container collection.
Emulsion particle diameter size and distribution are measured using dynamic light scattering method, as a result as shown in figure 1, average diameterd i
For 81 nm, polydispersity coefficient PDI is 0.29, and by the stability test of at least 1 week, the nanoemulsions were stable 100
Below nm, drop is without obvious roughening and lamination.
Take 4.5,9,18,36,100 mg PLGA- respectively in the same wayb- PEG repeats above-mentioned experiment, and the elapsed time is steady
Qualitative test, as shown in Figure 2, it is known that use 9 mg（I.e. 0.09 part）Above PLGA-b- PEG, obtaining nanometer aqueous emulsion can stablize
In below 200nm at least one month.
Example two：The preparation method contrast experiment of stirring and microcavity body high speed jet mixing is added dropwise（Pyrethrin nanoscale
Aqueous emulsion contains 45 mg PLGA-PEG and 0.5 mL pyrethrosin primary medicines）
Stirring contrast experiment is added dropwise：45 mg PLGA-PEG and 0.5 mL pyrethrosin primary medicines is taken to be dissolved in 4.5 mL acetone, by 5
ML water is slowly dropped into organic solution, is dripped off under 800rpm stirring conditions in 2 hours, prepares 10mL pyrethrins nanometer
Level aqueous emulsion.
The breast of the stability test, as shown in Figure 3 dropwise addition stirring to obtain of 1 week is carried out to suspending agent with dynamic light scattering method
Liquid, drop initial particle about 150nm is less than 100nm great Xu than what the method by microcavity body high speed jet mixing was obtained
It is many, increase to about 200nm by 1 day, occur in that obvious particle diameter roughening, less stable.
Example three：Different preparation methods（Stirring and microcavity body high speed jet mixing is added dropwise）Obtained pyrethrin water emulsion with
Commercially available pyrethrin water emulsion insecticidal effect contrast
Prepared by pyrethrin water emulsion, dropwise addition paddling process prepared by the difference microcavity body high speed jet mixing method of use example two
Pyrethrin water emulsion and certain commercially available best seller brand pyrethrin water emulsion be diluted to 5000 ppm and one respectively sprayed to drosophila
Secondary, its death condition and time are listed in the table below.
As a result show to be much better than to be added dropwise by the desinsection action speed of the pyrethrin nanometer aqueous emulsion prepared by the present invention
Pyrethrin water emulsion prepared by paddling process, and certain commercially available best seller brand pyrethrin water emulsion.
Claims (7)
1. a kind of highly effective and safe pyrethrin nanometer aqueous emulsion, it is characterised in that：By pyrethrin, emulsifying agent, acetone and water group
Into.
2. pyrethrin nanometer aqueous emulsion according to claim 1, it is characterised in that：The pyrethrin, emulsifying agent, third
Ketone, the volume ratio of water are 1: 0.018~0.2: 9: 10.
3. pyrethrin nanometer aqueous emulsion according to claim 1, it is characterised in that：The emulsifying agent is amphipathic block
Copolymer p LGA-b-PEG。
4. the preparation method of pyrethrin nanometer aqueous emulsion as claimed in claim 1, it is characterised in that：By pyrethrosin primary medicine
It is dissolved in emulsifying agent in acetone as oil phase, using water as aqueous phase, by aqueous phase and oil phase in microcavity body high speed jet mixing, system
Obtain pyrethrin nanometer aqueous emulsion.
5. the preparation method of pyrethrin nanometer aqueous emulsion according to claim 4, it is characterised in that：The Dalmatian chrysanthemum
The volume ratio of element, emulsifying agent and acetone is 1: 0.018~0.2: 9: 10.
6. the preparation method of the pyrethrin nanometer aqueous emulsion according to claim 4 or 5, it is characterised in that：The microcavity
The Reynolds number sum of each jet inlet is more than 2200 in body, and microcavity body volume is less than 0.1 mL.
7. the preparation method of pyrethrin nanometer aqueous emulsion according to claim 4, it is characterised in that：The emulsifying agent is
Amphipathic nature block polymer PLGA-b-PEG。
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710525957.1A CN107136057A (en) | 2017-06-30 | 2017-06-30 | A kind of highly effective and safe pyrethrin nanometer aqueous emulsion and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710525957.1A CN107136057A (en) | 2017-06-30 | 2017-06-30 | A kind of highly effective and safe pyrethrin nanometer aqueous emulsion and preparation method thereof |
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| CN107136057A true CN107136057A (en) | 2017-09-08 |
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| CN201710525957.1A Pending CN107136057A (en) | 2017-06-30 | 2017-06-30 | A kind of highly effective and safe pyrethrin nanometer aqueous emulsion and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110651783A (en) * | 2018-06-28 | 2020-01-07 | 江苏龙灯化学有限公司 | Preparation method of pesticide liquid composition, pesticide liquid composition prepared based on preparation method and application of pesticide liquid composition |
| CN114145315A (en) * | 2021-12-29 | 2022-03-08 | 成都绿金生物科技有限责任公司 | Pyrethrum extract emulsion in water and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1530012A (en) * | 2003-03-17 | 2004-09-22 | 北京华京五方实用纳米科技开发有限公 | Bromohydropyrethrin emulsion and production thereof |
| CN101341875A (en) * | 2008-08-25 | 2009-01-14 | 严兵 | Water-based natural pyrethrin sanitary insecticide and preparation method thereof |
| US20130137578A1 (en) * | 2011-11-30 | 2013-05-30 | Dow Agrosciences Llc | Stable suspoemulsions comprising a plurality of agriculturally active ingredients |
| CN105148758A (en) * | 2015-08-20 | 2015-12-16 | 扬州大学 | Method for rapidly preparing nano-emulsion |
-
2017
- 2017-06-30 CN CN201710525957.1A patent/CN107136057A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1530012A (en) * | 2003-03-17 | 2004-09-22 | 北京华京五方实用纳米科技开发有限公 | Bromohydropyrethrin emulsion and production thereof |
| CN101341875A (en) * | 2008-08-25 | 2009-01-14 | 严兵 | Water-based natural pyrethrin sanitary insecticide and preparation method thereof |
| US20130137578A1 (en) * | 2011-11-30 | 2013-05-30 | Dow Agrosciences Llc | Stable suspoemulsions comprising a plurality of agriculturally active ingredients |
| CN105148758A (en) * | 2015-08-20 | 2015-12-16 | 扬州大学 | Method for rapidly preparing nano-emulsion |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110651783A (en) * | 2018-06-28 | 2020-01-07 | 江苏龙灯化学有限公司 | Preparation method of pesticide liquid composition, pesticide liquid composition prepared based on preparation method and application of pesticide liquid composition |
| CN114145315A (en) * | 2021-12-29 | 2022-03-08 | 成都绿金生物科技有限责任公司 | Pyrethrum extract emulsion in water and preparation method thereof |
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Application publication date: 20170908 |