CN105994345A - Efficient cyfluthrin nano-emulsion composition and preparation method thereof - Google Patents
Efficient cyfluthrin nano-emulsion composition and preparation method thereof Download PDFInfo
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- CN105994345A CN105994345A CN201610578695.0A CN201610578695A CN105994345A CN 105994345 A CN105994345 A CN 105994345A CN 201610578695 A CN201610578695 A CN 201610578695A CN 105994345 A CN105994345 A CN 105994345A
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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
- A01N53/00—Biocides, pest repellants or attractants, or plant growth regulators containing cyclopropane carboxylic acids or derivatives thereof
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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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- Dentistry (AREA)
- Pest Control & Pesticides (AREA)
- Agronomy & Crop Science (AREA)
- Zoology (AREA)
- Plant Pathology (AREA)
- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
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Abstract
The invention discloses an efficient cyfluthrin nano-emulsion composition and a preparation method thereof. The efficient cyfluthrin nano-emulsion composition is prepared from, by mass, a surfactant 6.6-10%, an oil phase 10-20%, efficient cyfluthrin 2.5%, eistilled water 70%-82%, wherein the total mass percentage is 100%. The obtained efficient cyfluthrin nano-emulsion composition has the advantages that the stability is good, the organic solvent consumption is low, and the composition is easy to operate and use in agricultural production and the like. The particle size of pharmaceutical liquid is 69-150 nm. The polydispersity index (PDI) is 0.15-0.048. By adopting a single factor method and a triangular coordinate diagram method and using the emulsion particle size, the polydispersity index (PDI) and water removing stability as evaluation indexes, the test quantity is reduced, and the test efficiency is improved.
Description
Technical field
The present invention relates to formulations of pesticide research field, be specifically related to a kind of betacyfluthrin nanoemulsions group
Compound and preparation method thereof.
Background technology
Owing to betacyfluthrin is slightly soluble in water, it is soluble in the organic solvents such as acetone, toluene, dimethylbenzene.
The betacyfluthrin pesticide sold on the market at present, is mostly cream, microemulsion, aqueous emulsion.This
A little dosage forms suffer from inevitable shortcoming.Although wherein but cream preparation has good wetting effect breast
Plant and environment can be produced and destroy by a large amount of organic solvents in oil formulation, uses and be easily generated medicine on plant
Evil;Although with water as main medium in microemulsion, but owing to betacyfluthrin itself is slightly soluble in the spy of water
Point, need to add substantial amounts of polar latent solvent in production process has certain harm to environment, and due to preparation
Its active constituent content of feature own is on the low side;Aqueous emulsion belongs to thermodynamic instability body owing to medicinal liquid particle diameter is excessive
System, therefore its poor stability, it is susceptible to the phenomenon of medicinal liquid layering, is difficult to preserve for a long time.
Nanoemulsions is a kind of particle diameter colloidal dispersion system between thick emulsion and microemulsion, and particle diameter is distributed
Between 20-200nm, nanoemulsions is uniformly dispersed compared with thick emulsion, and particle diameter is less, physical stability
Good;Compare with microemulsion, prepare nanoemulsions and be greatly saved the input amount of surfactant, tradition microemulsion
In agent, the content of surfactant is minimum to reach more than 30%, and have good moistening, sprawl, permeate,
The using values such as medicine carrying.
Traditional low-energy emulsification method prepares nanoemulsions needs first to draw the pseudoternary phase diagram of oil, water, emulsifying agent,
Phase boundray according to pseudoternary phase diagram determines three Phase Proportion, carries out granularity again, stablizes after determining three Phase Proportion
Property measure.Wherein for determining that pseudoternary phase diagram phase boundray is accomplished by carrying out test in a large number, repeatedly, time-consuming take
Power.
Summary of the invention
For solve the problems referred to above, the present invention with single_factor method, triangle-coordinate figure as method, with emulsion particle diameter,
Polydispersity coefficient (PDI), to remove water stability be that evaluation index configures a kind of medicine stability profit good, biological
Expenditure betacyfluthrin nanoemulsions high, environment amenable.
For achieving the above object, the technical scheme that the present invention takes is:
A kind of betacyfluthrin nano-emulsion composition, by the component preparation of following mass percent
Become:
Preferably, described oil phase uses nontoxic non-irritating liquid paraffin.
Preferably, described surfactant is the mixture of Span80 and Tween80, Span80, Tween80
Mass ratio be Span80: Tween80=37%: 63%.
The preparation method of above-mentioned a kind of betacyfluthrin nano-emulsion composition, comprises the steps:
S1,2.5 mass parts betacyfluthrins are dissolved in the oil phase of 10 parts, be heated up to 65 DEG C
150rpm rotating speed stirs 15 minutes until solution clarification, obtains solution A;
S2, in solution A add 6.6-10 mass parts surfactant, obtain solution B;
S3,65 DEG C, under the rotating speed of 150rpm, by aqueous phase with 1mL/min-1Speed be added dropwise to emulsion B
In, obtaining betacyfluthrin nano-emulsion composition, room temperature preserves.
The method have the advantages that
Gained betacyfluthrin nano-emulsion composition has good stability, and consumption of organic solvent is few,
The advantage such as easily operated use in agricultural production, medicinal liquid particle diameter is 69-150nm (nanoemulsions desirable particle size
At below 200nm).Coefficient of dispersion PDI is 0.15-0.048 (the desirable particle size coefficient of dispersion less than 0.2);
With single_factor method, triangle-coordinate figure as method, with emulsion particle diameter, polydispersity coefficient (PDI), anhydrate surely
Qualitative for evaluation index configure, reduce tested number, improve test efficiency.
Accompanying drawing explanation
Fig. 1 is screening oil, water, Surfactant Ratio triaxial chart in the embodiment of the present invention.
Fig. 2 is oil phase in the embodiment of the present invention, aqueous phase, surfactant three-phase preferred communication area.
Detailed description of the invention
In order to make objects and advantages of the present invention clearer, below in conjunction with embodiment, the present invention is carried out
Further describe.Should be appreciated that specific embodiment described herein only in order to explain the present invention,
It is not intended to limit the present invention.
Embodiment 1
The preparation of betacyfluthrin nano-emulsion composition A
Nanoemulsions is in terms of 100 weight portions, and component is as follows: liquid white beeswax 10g, betacyfluthrin 2.5g,
Span80 3.7g, Tween80 6.3g, excess water is supplied.
Preparation process is as follows:
1, liquid paraffin 10g is mixed with betacyfluthrin 2.5g, be heated up to 65 ° at 150rpm
Rotating speed stirs 15 minutes until solution is clarified.
2, in oil item, add 3.7g Span80 and 6.3g Tween80, stir with 150rpm rotating speed
Mix.
3,65 DEG C, with the speed of 1ml/min-1,80g water droplet added oil item under the rotating speed of 150rpm,
Continue to carry out with the mixing speed of 150rmp the stirring of 15 minutes after filling up.I.e. can obtain the nano-emulsion of clarification
Liquid.
Embodiment 2
The preparation of betacyfluthrin nano-emulsion composition B
Nanoemulsions is in terms of 100 weight portions, and component is as follows: liquid white beeswax 20g, betacyfluthrin 2.5g,
Span80 3.7g, Tween80 6.3g, excess water is supplied.
Preparation process is as follows:
1, liquid paraffin 20g is mixed with betacyfluthrin 2.5g, be heated up to 65 ° at 150rpm
Rotating speed stirs 15 minutes until solution is clarified.
2, in oil item, add 3.7g Span80 and 6.3g Tween80, stir with 150rpm rotating speed
Mix.
3,65 DEG C, with the speed of 1ml/min-1,80g water droplet added oil item under the rotating speed of 150rpm,
Continue to carry out with the mixing speed of 150rmp the stirring of 15 minutes after filling up.I.e. can obtain the nano-emulsion of clarification
Liquid.
Embodiment 3
The preparation of 2.5% betacyfluthrin nano-emulsion composition E
Nanoemulsions is in terms of 100 weight portions, and component is as follows: liquid white beeswax 10g, betacyfluthrin 2.5g,
Span80 7.4g, Tween80 12.6g, excess water is supplied.
Preparation process is as follows:
1, liquid paraffin 20g is mixed with betacyfluthrin 2.5g, be heated up to 65 ° at 150rpm
Rotating speed stirs 15 minutes until solution is clarified.
2, in oil item, add 7.4g Span80 and 12.6g Tween80, stir with 150rpm rotating speed
Mix.
3,65 DEG C, with the speed of 1ml/min-1,80g water droplet added oil item under the rotating speed of 150rpm,
Continue to carry out with the mixing speed of 150rmp the stirring of 15 minutes after filling up.I.e. can obtain the nano-emulsion of clarification
Liquid.
Embodiment 4
The preparation of 2.5% betacyfluthrin nano-emulsion composition G
Nanoemulsions is in terms of 100 weight portions, and component is as follows: liquid white beeswax 10 parts, betacyfluthrin
2.5g, 2.442g Span80,4.158g Tween80, excess water is supplied.
Preparation process is as follows:
1, liquid paraffin 10g is mixed with betacyfluthrin 2.5g, be heated up to 65 ° at 150rpm
Rotating speed stirs 15 minutes until solution is clarified.
2, in oil item, add 2.442g Span80 and 4.158g Tween80, enter with 150rpm rotating speed
Row stirring.
3,65 DEG C, with the speed of 1ml/min-1,80g water droplet added oil item under the rotating speed of 150rpm,
Continue to carry out with the mixing speed of 150rmp the stirring of 15 minutes after filling up.I.e. can obtain the nano-emulsion of clarification
Liquid.
Aqueous emulsion hydrophile-lipophile balance value screening in table 1 betacyfluthrin nanoemulsions
As can be known from Table 1, when the 5th group of test HLB value is 11, it is two kinds of surfactant optimum proportioning.
Table 2 betacyfluthrin nanoemulsions oil, water, surfactant three Phase Proportion the selection result
As can be known from Table 2, when emulsifying agent HLB is 11, surfactant, oil phase, aqueous phase three Phase Proportion
Screening, the formula G coefficient of dispersion is minimum, and emulsifying agent, liquid paraffin consumption is minimum, cost is minimum, for most preferably
Formula.Particle diameter, the coefficient of dispersion, all much smaller than comparison medicament, illustrate that this dosage form is more stable than comparison medicament, unsuitable
Layering occurs.
With single_factor method, triangle-coordinate figure (as depicted in figs. 1 and 2) as method, with emulsion particle diameter,
Polydispersity coefficient (PDI), go water stability be evaluation index configuration, reduce tested number, improve test
Efficiency.
Triangle-coordinate figure refers to set up with the content of 3 kinds of components for coordinate in an equilateral triangle sit
Mark system, by examination experimental index, the method finally determining 3 kinds of component optimum proportioning.Though in the triangles
There is a lot of point, but start only need to select to do several point having representative, then want according to the examination of experimental index
Asking the region determining better formula place, in this region, screening can obtain optimal proportioning further.
In equilateral triangle Fig. 1, owing to this nanoemulsions beforehand research target is oil-in-water type nanoemulsions.For
Reduce tested number, and phase transformation law can be embodied, aqueous phase is set to more than 50%, simultaneously for reducing cost crude
Need the content more than or equal to surfactant mutually, additionally by pre-stage test, find the efficient cyfluthrin of 2.5g
Chrysanthemum ester will dissolving faster at a temperature of 65 DEG C, at least need 10g liquid paraffin.Therefore Fig. 1 is selected
Upper 5 points, carry out ratio screening.
The above is only the preferred embodiment of the present invention, it is noted that common for the art
For technical staff, under the premise without departing from the principles of the invention, it is also possible to make some improvements and modifications,
These improvements and modifications also should be regarded as protection scope of the present invention.
Claims (4)
1. a betacyfluthrin nano-emulsion composition, it is characterised in that by following percent mass
The component of ratio is prepared from:
A kind of betacyfluthrin nano-emulsion composition the most according to claim 1, its feature
Being, described oil phase uses nontoxic non-irritating liquid paraffin.
A kind of betacyfluthrin nano-emulsion composition the most according to claim 1, its feature
Being, described surfactant is the mixture of Span80 and Tween80, Span80, Tween80's
Mass ratio is Span80: Tween80=37%: 63%.
4. the preparation method of a betacyfluthrin nano-emulsion composition, it is characterised in that include
Following steps:
S1,2.5 mass parts betacyfluthrins are dissolved in the oil phase of 10 parts, be heated up to 65 DEG C
150rpm rotating speed stirs 15 minutes until solution clarification, obtains solution A;
S2, in solution A add 6.6-10 mass parts surfactant, obtain solution B;
S3,65 DEG C, under the rotating speed of 150rpm, by aqueous phase with 1mL/min-1Speed be added dropwise to emulsion B
In, obtaining betacyfluthrin nano-emulsion composition, room temperature preserves.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109463382A (en) * | 2018-10-10 | 2019-03-15 | 安徽农业大学 | Using tea saponin as the pesticidal nanoemulsion and preparation method of surfactant |
CN110973152A (en) * | 2019-11-12 | 2020-04-10 | 南京华洲药业有限公司 | High-efficiency cypermethrin nano water aqua and preparation method and application thereof |
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Non-Patent Citations (2)
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109463382A (en) * | 2018-10-10 | 2019-03-15 | 安徽农业大学 | Using tea saponin as the pesticidal nanoemulsion and preparation method of surfactant |
CN109463382B (en) * | 2018-10-10 | 2021-06-22 | 安徽久易农业股份有限公司 | Insecticidal nano-emulsion taking tea saponin as surfactant and preparation method thereof |
CN110973152A (en) * | 2019-11-12 | 2020-04-10 | 南京华洲药业有限公司 | High-efficiency cypermethrin nano water aqua and preparation method and application thereof |
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