CN106259335A - A kind of rosin acid sodium microemulsion - Google Patents
A kind of rosin acid sodium microemulsion Download PDFInfo
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- CN106259335A CN106259335A CN201610626213.4A CN201610626213A CN106259335A CN 106259335 A CN106259335 A CN 106259335A CN 201610626213 A CN201610626213 A CN 201610626213A CN 106259335 A CN106259335 A CN 106259335A
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- Prior art keywords
- microemulsion
- acid sodium
- ether
- rosin acid
- surfactant
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N37/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids
- A01N37/08—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids containing carboxylic groups or thio analogues thereof, directly attached by the carbon atom to a cycloaliphatic ring; Derivatives thereof
-
- 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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- Life Sciences & Earth Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Health & Medical Sciences (AREA)
- Pest Control & Pesticides (AREA)
- Agronomy & Crop Science (AREA)
- Plant Pathology (AREA)
- Engineering & Computer Science (AREA)
- Dentistry (AREA)
- Wood Science & Technology (AREA)
- Zoology (AREA)
- Environmental Sciences (AREA)
- Dispersion Chemistry (AREA)
- Chemical & Material Sciences (AREA)
- Toxicology (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The present invention relates to a kind of rosin acid sodium microemulsion, it is made up of following component and weight percentage thereof: rosin acid sodium 5 20%, surfactant 2 20%, solvent 2 10%, cosolvent 2 10%, defoamer 0.1 5%, antifreezing agent 0.1 5%, water supplies 100%.
Description
Technical field
The present invention relates to agriculture field, be specifically related to a kind of rosin acid sodium microemulsion, and the preparation side of described microemulsion
Method.
Background technology
Rosin acid sodium Emulsion is a kind of novel pesticide based on natural material, and it has good fat-soluble, one-tenth
Film and emulsifiability.Current main dosage form includes cream, soluble powder, soluble granula, water dispersible granules etc..
CN103314957A discloses a kind of rosin acid sodium water dispersible granules, and it includes rosin acid sodium soluble powder, takes off
Sugar sodium lignin sulfonate, sodium sulfate, filler or dispersant and adhesion promoter.
CN1903042A discloses a kind of rosin acid sodium soluble powder preparation method, high including pinaster body carries out high temperature
Pressure processes, and then vapour oil-water separation carry out Colophonium purification, eventually passes saponification process, moisture evaporate, dry, crush, and obtaining can
Dissolubility powder.
CN104705333A discloses a kind of containing rosin acid sodium with the Pesticidal combination of sulfoxaflor, has including first
Imitate composition rosin acid sodium and the second effective ingredient sulfoxaflor and conventional auxiliary element, rosin acid sodium and sulfoxaflor
Ratio of weight and number is 50: 1-1: 1, and rosin acid sodium with sulfoxaflor weight summation percentage by weight in Pesticidal combination is
5%-60%.
Microemulsion is a kind of formulations of pesticide, belong to thermodynamics through time stable dispersion, it is with water as medium, saves big
Amount organic solvent, does not fire the most quick-fried, production operation, storing safe, low in the pollution of the environment.
The existing Emulsion of rosin acid sodium is susceptible to layering and decomposing phenomenon during storing, and the present inventor is existing for overcoming
There is the drawbacks described above of technology, by substantial amounts of test, have developed rosin acid sodium microemulsion, its good stability, every quality index
Excellent.Being based on above-mentioned discovery, inventor completes the present invention.
Summary of the invention
The technical problem to be solved is to provide a kind of stable rosin acid sodium microemulsion.In order to solve above-mentioned asking
Topic, the present invention uses following technical scheme.
One aspect of the present invention relates to a kind of rosin acid sodium microemulsion, and it is made up of following component and weight percentage thereof:
Rosin acid sodium 5-20%
Surfactant 2-20%
Solvent 2-10%
Cosolvent 2-10%
Defoamer 0.1-5%
Antifreezing agent 0.1-5%
Water supplies 100%.
Preferably, each component and weight percentage thereof are:
Rosin acid sodium 8-15%
Surfactant 7-18%
Solvent 3-8%
Cosolvent 3-6%
Defoamer 0.5-2%
Antifreezing agent 03-4%
Water supplies 100%.
It is highly preferred that each component and weight percentage thereof are:
Rosin acid sodium 10-12%
Surfactant 9-14%
Solvent 5-7%
Cosolvent 4-5%
Defoamer 0.5-1%
Antifreezing agent 2-4%
Water supplies 100%.
In formula of the present invention, wherein,
Described surfactant is selected from NONIN HS 240, tributyl phenyl polyglycol ether, polyoxyethylene mountain
One or more in pears alcohol fatty acid ester, dioctyl sodium sulphosuccinate, polyoxyethylene lauryl ether sodium acetate.
Preferably, described surfactant is selected from tributyl phenyl polyglycol ether, polyoxyethylene lauryl ether sodium acetate
In one or both.
It is highly preferred that described surfactant is tributyl phenyl polyglycol ether and polyoxyethylene lauryl ether sodium acetate
Mixture, the weight ratio of the two is 1: 5 to 5: 1, preferably 1: 3 to 3: 1, such as 1: 3,1: 2,1: 1,2: 1,3: 1, most preferably
2∶1。
Described solvent selected from acetone, toluene, chloroform, dimethylformamide, hexamethylene, Propylene Glycol ether, diformazan
One or more in base sulfoxide, petroleum ether.It is preferably one or more in acetone, dimethylformamide, dimethyl sulfoxide.
One or more in ethanol, isopropanol, n-butyl alcohol, isobutanol, isoamyl alcohol of described cosolvent.The most different
One or more in propanol, n-butyl alcohol, isoamyl alcohol.
Described defoamer is selected from n-octyl alcohol, polydimethylsiloxane, polypropylene glycerol aether, butylphosphoric acid ester, phosphoric acid isobutyl
One or more in ester, silicone.
One or more in ethylene glycol, glycerol, propylene glycol, Polyethylene Glycol or sorbitol of described antifreezing agent.
Another aspect of the present invention relates to the preparation method of described rosin acid sodium microemulsion, and it mainly comprises the steps of,
(1) by solvent and cosolvent mix homogeneously, add rosin acid sodium afterwards, and stir, obtain oil phase；Wherein stir
Mixing speed and can be 100-1000 rev/min, mixing time is 30-60 minute；
(2) surfactant, defoamer, antifreezing agent are added to the water, and stir, obtain aqueous phase；Wherein stir speed
Degree can be 100-1000 rev/min, and mixing time is 15-30 minute；
(3) oil phase step (1) obtained while stirring adds in the aqueous phase that step (2) obtains, and continues stirring, stirring speed
Degree can be 100-1000 rev/min, and mixing time is 15-40 minute, makes microemulsion.
The rosin acid sodium microemulsion good stability that the present invention obtains, every quality index is excellent, and insecticidal effect significantly improves.
Detailed description of the invention
In order to understand the present invention, further illustrate the present invention with embodiment below, but be not intended to the present invention.
(1) example of formulations
In following example of formulations, unless otherwise indicated, described percentage ratio is all weight percentage.
Embodiment 1
Rosin acid sodium 8%, tributyl phenyl polyglycol ether 11%, dimethylformamide 5%, isopropanol 4%, poly-diformazan
Radical siloxane 0.5%, ethylene glycol 3%, water supplies 100%.
By solvent and cosolvent mix homogeneously, add rosin acid sodium afterwards, stir 40 minutes with the rotating speeds of 200 revs/min,
To oil phase.Surfactant, defoamer, antifreezing agent are added to the water, stir 25 minutes with the rotating speeds of 300 revs/min, obtain water
Phase.While stirring oil phase is added in aqueous phase, continue stirring 30 minutes with the rotating speeds of 300 revs/min, make microemulsion.
Embodiment 2
Rosin acid sodium 15%, polyoxyethylene lauryl ether sodium acetate 18%, dimethyl sulfoxide 8%, n-butyl alcohol 6%, polyoxy
Propylene glycerin ether 1%, propylene glycol 4%, water supplies 100%.
By solvent and cosolvent mix homogeneously, add rosin acid sodium afterwards, stir 40 minutes with the rotating speeds of 200 revs/min,
To oil phase.Surfactant, defoamer, antifreezing agent are added to the water, stir 25 minutes with the rotating speeds of 300 revs/min, obtain water
Phase.While stirring oil phase is added in aqueous phase, continue stirring 30 minutes with the rotating speeds of 300 revs/min, make microemulsion.
Embodiment 3
Rosin acid sodium 12%, tributyl phenyl polyglycol ether 8%, polyoxyethylene lauryl ether sodium acetate 4%, dimethyl
Sulfoxide 6%, isopropanol 5%, phosphoric acid isobutyl ester 1%, Polyethylene Glycol 4%, water supplies 100%.
By solvent and cosolvent mix homogeneously, add rosin acid sodium afterwards, stir 40 minutes with the rotating speeds of 200 revs/min,
To oil phase.Surfactant, defoamer, antifreezing agent are added to the water, stir 25 minutes with the rotating speeds of 300 revs/min, obtain water
Phase.While stirring oil phase is added in aqueous phase, continue stirring 30 minutes with the rotating speeds of 300 revs/min, make microemulsion.
Embodiment 4
Rosin acid sodium 6%, tributyl phenyl polyglycol ether 2%, polyoxyethylene lauryl ether sodium acetate 6%, acetone
4%, isopropanol 3%, silicone 0.5%, glycerol 2%, water supplies 100%.
By solvent and cosolvent mix homogeneously, add rosin acid sodium afterwards, stir 40 minutes with the rotating speeds of 200 revs/min,
To oil phase.Surfactant, defoamer, antifreezing agent are added to the water, stir 25 minutes with the rotating speeds of 300 revs/min, obtain water
Phase.While stirring oil phase is added in aqueous phase, continue stirring 30 minutes with the rotating speeds of 300 revs/min, make microemulsion.
Comparative example 1
Rosin acid sodium 12%, fatty alcohol-polyoxyethylene ether 8%, calcium dodecyl benzene sulfonate 4%, dimethyl sulfoxide 6%, different
Propanol 5%, phosphoric acid isobutyl ester 1%, Polyethylene Glycol 4%, water supplies 100%.
By solvent and cosolvent mix homogeneously, add rosin acid sodium afterwards, stir 40 minutes with the rotating speeds of 200 revs/min,
To oil phase.Surfactant, defoamer, antifreezing agent are added to the water, stir 25 minutes with the rotating speeds of 300 revs/min, obtain water
Phase.While stirring oil phase is added in aqueous phase, continue stirring 30 minutes with the rotating speeds of 300 revs/min, make microemulsion.
Comparative example 2
Rosin acid sodium 8%, sodium lignin sulfonate 11%, dimethylformamide 5%, isopropanol 4%, polydimethylsiloxane
0.5%, ethylene glycol 3%, water supplies 100%.
By solvent and cosolvent mix homogeneously, add rosin acid sodium afterwards, stir 40 minutes with the rotating speeds of 200 revs/min,
To oil phase.Surfactant, defoamer, antifreezing agent are added to the water, stir 25 minutes with the rotating speeds of 300 revs/min, obtain water
Phase.While stirring oil phase is added in aqueous phase, continue stirring 30 minutes with the rotating speeds of 300 revs/min, make microemulsion.
(2) determination of quality index
1, low-temperature stability measures
According to GB-T 19137-2003, the low-temperature stability of invention formulation is measured.It is specially sample at 0 DEG C
After storing 14 days, observe its cosmetic variation.Result see table.
Table 1 low-temperature stability measures
| Sample | Result |
| Embodiment 1 | The most unchanged |
| Embodiment 2 | The most unchanged |
| Embodiment 3 | Unchanged |
| Embodiment 4 | Unchanged |
| Comparative example 1 | Emulsion is muddy, has lamination |
| Comparative example 2 | Emulsion is muddy, has lamination |
Result shows, inventive samples is after cold storage, and outward appearance is the most unchanged.Control sample then emulsion is muddy, has
Lamination.
2, heat storage stability measures
According to GB-T 19136-2003, the heat storage stability of invention formulation is measured.It is specially and sample is placed in
In ampere bottle, after 54 DEG C are stored 14 days, observe outward appearance and also measure active component content, calculate resolution ratio.Result see table.
Table 2 heat storage stability measures
| Sample | Outward appearance | Resolution ratio |
| Embodiment 1 | The most unchanged | 2.7% |
| Embodiment 2 | The most unchanged | 2.5% |
| Embodiment 3 | Unchanged | 0.8% |
| Embodiment 4 | Unchanged | 1.1% |
| Comparative example 1 | Layering | 9.5% |
| Comparative example 2 | Layering | 8.4% |
Result shows, after overheated storage, inventive samples outward appearance is the most unchanged, and resolution ratio is relatively low, especially implements
Example 3-4 sample, almost without decomposition.By contrast, there is layering in control sample, and active ingredient breaks down rate is higher.
3, stability of emulsion measures
According to GB/T 1603-2001, the stability of emulsion of invention formulation is measured.Specifically, at 250ml beaker
In, add the standard hard water of 100ml 30 DEG C, with pipette, extract 1ml microemulsion sample, move in graduated cylinder after stirring, and
Graduated cylinder is placed in 30 DEG C of waters bath with thermostatic control, stands 1 hour, observe emulsion separation situation.Result is as follows.
Table 3 stability of emulsion measures
| Sample | Result |
| Embodiment 1 | Upper without oil slick, lower without precipitation, clear |
| Embodiment 2 | Upper without oil slick, lower without precipitation, clear |
| Embodiment 3 | Upper without oil slick, lower without precipitation, clear |
| Embodiment 4 | Upper without oil slick, lower without precipitation, clear |
| Comparative example 1 | On have an oil slick, emulsion is muddy |
| Comparative example 2 | On have an oil slick, emulsion is muddy |
Result shows, without oil slick in emulsion after inventive samples 1 hour, lower without precipitating, clear.And control sample
Then produce oil slick on emulsion surface, emulsion is muddy.
(3) field control effectiveness test
The test invention formulation prevention effect to cotton aphid.
Select aphid that consistent Cotton Gossypii plot, division of cells occur, carry out insect population radix investigation before medicine.Spray the most respectively
Embodiment of the present invention 1-4 and the medicament of comparative example 1-2.Each process dosage is consistent, and control is 25 active component/mu, often processes 3
Secondary repetition.Fresh water spraying is comparison.5 days survey results after medicine, calculate preventive effect.Result see table
Table 4 field efficacy measures
| Medicament | Preventive effect |
| Embodiment 1 | 88.3% |
| Embodiment 2 | 85.5% |
| Embodiment 3 | 94.5% |
| Embodiment 4 | 91.8% |
| Comparative example 1 | 62.6% |
| Comparative example 2 | 67.2% |
| Clear water compares | - |
Result shows, the preventive effect of cotton aphid, relative to control formulation, is significantly improved by invention formulation.
Examples detailed above is only that the present invention is explained further, and is not limitation of the invention, by by above-mentioned side
The scheme that case simply adjusts and then obtains, equally within the protection domain of the application.
Claims (10)
1. a rosin acid sodium microemulsion, it is made up of following component and weight percentage thereof:
Rosin acid sodium 5-20%
Surfactant 2-20%
Solvent 2-10%
Cosolvent 2-10%
Defoamer 0.1-5%
Antifreezing agent 0.1-5%
Water supplies 100%.
Microemulsion the most according to claim 1, it is characterised in that each component and weight percentage thereof be:
Rosin acid sodium 8-15%
Surfactant 7-18%
Solvent 3-8%
Cosolvent 3-6%
Defoamer 0.5-2%
Antifreezing agent 0.5-4%
Water supplies 100%.
Microemulsion the most according to claim 1 and 2, it is characterised in that described surfactant is selected from polyoxethylene octylphenyl
Phenyl ether, tributyl phenyl polyglycol ether, Polyoxyethylene Sorbitol Fatty Acid Esters, dioctyl sodium sulphosuccinate, lauryl alcohol
One or more in polyethenoxy ether acetic acid sodium.
Microemulsion the most according to claim 3, it is characterised in that described surfactant is selected from the poly-second of tributyl phenyl two
One or both in alcohol ether, polyoxyethylene lauryl ether sodium acetate.
Microemulsion the most according to claim 4, it is characterised in that described surfactant is tributyl phenyl Polyethylene Glycol
Ether and the mixture of polyoxyethylene lauryl ether sodium acetate.
Microemulsion the most according to claim 1 and 2, it is characterised in that described solvent selected from acetone, toluene, chloroform,
One or more in dimethylformamide, hexamethylene, Propylene Glycol ether, dimethyl sulfoxide, petroleum ether.
Microemulsion the most according to claim 1 and 2, it is characterised in that described cosolvent is selected from ethanol, isopropanol, positive fourth
One or more in alcohol, isobutanol, isoamyl alcohol.
Microemulsion the most according to claim 1 and 2, it is characterised in that described defoamer is selected from n-octyl alcohol, poly dimethyl silicon
One or more in oxygen alkane, polypropylene glycerol aether, butylphosphoric acid ester, phosphoric acid isobutyl ester, silicone.
Microemulsion the most according to claim 1 and 2, it is characterised in that described antifreezing agent selected from ethylene glycol, glycerol, third
One or more in glycol, Polyethylene Glycol or sorbitol.
10. the preparation method of microemulsion described in an any one of claim 1-9, it is characterised in that comprise the steps of,
(1) by solvent and cosolvent mix homogeneously, add rosin acid sodium afterwards, and stir, obtain oil phase；
(2) surfactant, defoamer, antifreezing agent are added to the water, and stir, obtain aqueous phase；
(3) oil phase step (1) obtained while stirring adds in the aqueous phase that step (2) obtains, and continues stirring, makes microemulsion
Agent.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110312831A (en) * | 2016-11-17 | 2019-10-08 | 北欧生物技术集团有限公司 | Prepare the method with the fibrous material of anti-microbial properties |
| WO2019220011A1 (en) * | 2018-05-16 | 2019-11-21 | Nordic Biotech Group Oy | An antimicrobial composition |
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| WO2003064500A2 (en) * | 2002-01-25 | 2003-08-07 | Dow Corning Corporation | Compositions containing silicone oil-in-water emulsions, salts, alcohols and solvents |
| CN103314957A (en) * | 2013-03-27 | 2013-09-25 | 浙江工业大学 | Sodium abietate insecticide and preparation method thereof |
| CN104757018A (en) * | 2015-03-23 | 2015-07-08 | 苏州谷力生物科技有限公司 | Pesticide composition |
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2016
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| WO2003064500A2 (en) * | 2002-01-25 | 2003-08-07 | Dow Corning Corporation | Compositions containing silicone oil-in-water emulsions, salts, alcohols and solvents |
| CN103314957A (en) * | 2013-03-27 | 2013-09-25 | 浙江工业大学 | Sodium abietate insecticide and preparation method thereof |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110312831A (en) * | 2016-11-17 | 2019-10-08 | 北欧生物技术集团有限公司 | Prepare the method with the fibrous material of anti-microbial properties |
| JP2020502375A (en) * | 2016-11-17 | 2020-01-23 | ノルディック バイオテック グループ オサケ ユキチュアＮｏｒｄｉｃ Ｂｉｏｔｅｃｈ Ｇｒｏｕｐ Ｏｙ | Method of producing fibrous material having antimicrobial properties |
| EP3541987A4 (en) * | 2016-11-17 | 2020-05-27 | Nordic Biotech Group OY | Process for producing fibrous material with antimicrobial properties |
| JP7081834B2 (en) | 2016-11-17 | 2022-06-07 | ノルディック バイオテック グループ オサケ ユキチュア | Method for manufacturing fibrous material with antimicrobial properties |
| US11598047B2 (en) | 2016-11-17 | 2023-03-07 | Nordic Biotech Group Oy | Process for producing fibrous material with antimicrobial properties |
| WO2019220011A1 (en) * | 2018-05-16 | 2019-11-21 | Nordic Biotech Group Oy | An antimicrobial composition |
| CN112236037A (en) * | 2018-05-16 | 2021-01-15 | 北欧生物技术集团有限公司 | Antimicrobial compositions |
| JP2021524847A (en) * | 2018-05-16 | 2021-09-16 | ノルディック バイオテック グループ オサケ ユキチュアＮｏｒｄｉｃ Ｂｉｏｔｅｃｈ Ｇｒｏｕｐ Ｏｙ | Antimicrobial composition |
| EP3793359A4 (en) * | 2018-05-16 | 2022-03-09 | Nordic Biotech Group Oy | An antimicrobial composition |
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