CN106259335B - A kind of rosin acid sodium microemulsion - Google Patents
A kind of rosin acid sodium microemulsion Download PDFInfo
- Publication number
- CN106259335B CN106259335B CN201610626213.4A CN201610626213A CN106259335B CN 106259335 B CN106259335 B CN 106259335B CN 201610626213 A CN201610626213 A CN 201610626213A CN 106259335 B CN106259335 B CN 106259335B
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- Prior art keywords
- acid sodium
- rosin acid
- revs
- minutes
- microemulsion
- Prior art date
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- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 title claims abstract description 38
- RSWGJHLUYNHPMX-ONCXSQPRSA-N abietic acid Chemical compound C([C@@H]12)CC(C(C)C)=CC1=CC[C@@H]1[C@]2(C)CCC[C@@]1(C)C(O)=O RSWGJHLUYNHPMX-ONCXSQPRSA-N 0.000 title claims abstract description 38
- 239000011734 sodium Substances 0.000 title claims abstract description 38
- 229910052708 sodium Inorganic materials 0.000 title claims abstract description 38
- 239000004530 micro-emulsion Substances 0.000 title claims abstract description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000004094 surface-active agent Substances 0.000 claims abstract description 15
- 239000002518 antifoaming agent Substances 0.000 claims abstract description 13
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 13
- 239000006184 cosolvent Substances 0.000 claims abstract description 13
- 239000002904 solvent Substances 0.000 claims abstract description 13
- 239000012071 phase Substances 0.000 claims description 24
- -1 tributyl phenyl Chemical group 0.000 claims description 22
- 239000003921 oil Substances 0.000 claims description 19
- 238000003756 stirring Methods 0.000 claims description 19
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 18
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 12
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 10
- 239000008346 aqueous phase Substances 0.000 claims description 7
- 229920000151 polyglycol Polymers 0.000 claims description 7
- 239000010695 polyglycol Substances 0.000 claims description 7
- 239000001632 sodium acetate Substances 0.000 claims description 7
- 235000017281 sodium acetate Nutrition 0.000 claims description 7
- 239000002202 Polyethylene glycol Substances 0.000 claims description 4
- 229920001223 polyethylene glycol Polymers 0.000 claims description 4
- 238000002360 preparation method Methods 0.000 claims description 4
- SVBLDLLXNRGMBG-UHFFFAOYSA-N 2-methylpropyl dihydrogen phosphate Chemical compound CC(C)COP(O)(O)=O SVBLDLLXNRGMBG-UHFFFAOYSA-N 0.000 claims description 3
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 11
- 239000000203 mixture Substances 0.000 description 10
- 239000000523 sample Substances 0.000 description 10
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 9
- 238000009472 formulation Methods 0.000 description 9
- 239000006210 lotion Substances 0.000 description 9
- DNIAPMSPPWPWGF-UHFFFAOYSA-N monopropylene glycol Natural products CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 8
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical group CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 7
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 6
- 239000000839 emulsion Substances 0.000 description 5
- 238000002156 mixing Methods 0.000 description 5
- 230000001376 precipitating effect Effects 0.000 description 5
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 4
- 239000005934 Sulfoxaflor Substances 0.000 description 4
- ZVQOOHYFBIDMTQ-UHFFFAOYSA-N [methyl(oxido){1-[6-(trifluoromethyl)pyridin-3-yl]ethyl}-lambda(6)-sulfanylidene]cyanamide Chemical compound N#CN=S(C)(=O)C(C)C1=CC=C(C(F)(F)F)N=C1 ZVQOOHYFBIDMTQ-UHFFFAOYSA-N 0.000 description 4
- 239000003814 drug Substances 0.000 description 4
- PHTQWCKDNZKARW-UHFFFAOYSA-N isoamylol Chemical compound CC(C)CCO PHTQWCKDNZKARW-UHFFFAOYSA-N 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 4
- 238000003860 storage Methods 0.000 description 4
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 239000013068 control sample Substances 0.000 description 3
- 238000005338 heat storage Methods 0.000 description 3
- 238000003475 lamination Methods 0.000 description 3
- 230000003449 preventive effect Effects 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- KBPLFHHGFOOTCA-UHFFFAOYSA-N 1-Octanol Chemical group CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 description 2
- 241001600408 Aphis gossypii Species 0.000 description 2
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 2
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 2
- YDEXUEFDPVHGHE-GGMCWBHBSA-L disodium;(2r)-3-(2-hydroxy-3-methoxyphenyl)-2-[2-methoxy-4-(3-sulfonatopropyl)phenoxy]propane-1-sulfonate Chemical compound [Na+].[Na+].COC1=CC=CC(C[C@H](CS([O-])(=O)=O)OC=2C(=CC(CCCS([O-])(=O)=O)=CC=2)OC)=C1O YDEXUEFDPVHGHE-GGMCWBHBSA-L 0.000 description 2
- 235000019441 ethanol Nutrition 0.000 description 2
- 235000011187 glycerol Nutrition 0.000 description 2
- ZXEKIIBDNHEJCQ-UHFFFAOYSA-N isobutanol Chemical compound CC(C)CO ZXEKIIBDNHEJCQ-UHFFFAOYSA-N 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 230000000361 pesticidal effect Effects 0.000 description 2
- 239000000575 pesticide Substances 0.000 description 2
- 229920001296 polysiloxane Polymers 0.000 description 2
- 229920005573 silicon-containing polymer Polymers 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 239000004562 water dispersible granule Substances 0.000 description 2
- RSWGJHLUYNHPMX-UHFFFAOYSA-N Abietic-Saeure Natural products C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 description 1
- 241001124076 Aphididae Species 0.000 description 1
- 229920000742 Cotton Polymers 0.000 description 1
- 239000001836 Dioctyl sodium sulphosuccinate Substances 0.000 description 1
- HSRJKNPTNIJEKV-UHFFFAOYSA-N Guaifenesin Chemical compound COC1=CC=CC=C1OCC(O)CO HSRJKNPTNIJEKV-UHFFFAOYSA-N 0.000 description 1
- 241000238631 Hexapoda Species 0.000 description 1
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 1
- 235000008331 Pinus X rigitaeda Nutrition 0.000 description 1
- 235000011613 Pinus brutia Nutrition 0.000 description 1
- 241000018646 Pinus brutia Species 0.000 description 1
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 1
- 241000220324 Pyrus Species 0.000 description 1
- KHPCPRHQVVSZAH-HUOMCSJISA-N Rosin Natural products O(C/C=C/c1ccccc1)[C@H]1[C@H](O)[C@@H](O)[C@@H](O)[C@@H](CO)O1 KHPCPRHQVVSZAH-HUOMCSJISA-N 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 239000002318 adhesion promoter Substances 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- OOCMUZJPDXYRFD-UHFFFAOYSA-L calcium;2-dodecylbenzenesulfonate Chemical compound [Ca+2].CCCCCCCCCCCCC1=CC=CC=C1S([O-])(=O)=O.CCCCCCCCCCCCC1=CC=CC=C1S([O-])(=O)=O OOCMUZJPDXYRFD-UHFFFAOYSA-L 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- 235000019329 dioctyl sodium sulphosuccinate Nutrition 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000002552 dosage form Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 150000002191 fatty alcohols Chemical class 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000013505 freshwater Substances 0.000 description 1
- 239000008233 hard water Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 230000000749 insecticidal effect Effects 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000000593 microemulsion method Methods 0.000 description 1
- 239000005445 natural material Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 235000021017 pears Nutrition 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-N phosphoric acid Substances OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 1
- 229940051841 polyoxyethylene ether Drugs 0.000 description 1
- 229920000056 polyoxyethylene ether Polymers 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000007127 saponification reaction Methods 0.000 description 1
- APSBXTVYXVQYAB-UHFFFAOYSA-M sodium docusate Chemical compound [Na+].CCCCC(CC)COC(=O)CC(S([O-])(=O)=O)C(=O)OCC(CC)CCCC APSBXTVYXVQYAB-UHFFFAOYSA-M 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 150000003462 sulfoxides Chemical class 0.000 description 1
- KHPCPRHQVVSZAH-UHFFFAOYSA-N trans-cinnamyl beta-D-glucopyranoside Natural products OC1C(O)C(O)C(CO)OC1OCC=CC1=CC=CC=C1 KHPCPRHQVVSZAH-UHFFFAOYSA-N 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
Classifications
-
- 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
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- 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)
- Zoology (AREA)
- Environmental Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Toxicology (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The present invention relates to a kind of rosin acid sodium microemulsions, are made of following component and its weight percentage: rosin acid sodium 5-20%, surfactant 2-20%, solvent 2-10%, cosolvent 2-10%, defoaming agent 0.1-5%, antifreezing agent 0.1-5%, water supply 100%.
Description
Technical field
The present invention relates to agriculture fields, and in particular to the preparation side of a kind of rosin acid sodium microemulsion and the microemulsion
Method.
Background technique
Rosin acid sodium emulsion is a kind of novel pesticide based on natural material, with it is good it is fat-soluble, at
Film property and emulsifiability.Current main dosage form includes missible oil, soluble powder, soluble granula, water dispersible granules etc..
CN103314957A discloses a kind of rosin acid sodium water dispersible granules comprising rosin acid sodium soluble powder takes off
Sugared sodium lignin sulfonate, sodium sulphate, filler or dispersing agent and adhesion promoter.
CN1903042A discloses a kind of rosin acid sodium soluble powder preparation method, including pine tree ontology is carried out high temperature height
Then pressure processing, vapour water-oil separating carry out rosin purification, finally evaporate, dry by saponification process, moisture, is broken, obtaining can
Dissolubility powder.
CN104705333A discloses a kind of Pesticidal combination containing rosin acid sodium and sulfoxaflor, including first has
Effect ingredient rosin acid sodium and the second effective component sulfoxaflor and common auxiliary element, rosin acid sodium and sulfoxaflor
Weight fraction ratio is 50: 1-1: 1, and rosin acid sodium is with weight percent of the sulfoxaflor weight summation in Pesticidal combination
5%-60%.
Microemulsion is a kind of formulations of pesticide, belong to thermodynamics through when stable dispersion save big using water as medium
Organic solvent is measured, non-ignitable not quick-fried, production operation, storing are safe, low in the pollution of the environment.
The existing emulsion of rosin acid sodium is easy to happen layering and decomposing phenomenon during storage, and the present inventor is to overcome now
There is the drawbacks described above of technology, by largely testing, have developed rosin acid sodium microemulsion, stability is good, every quality index
It is excellent.It is based on above-mentioned discovery, inventor completes the present invention.
Summary of the invention
Technical problem to be solved by the invention is to provide a kind of stable rosin acid sodium microemulsions.In order to solve above-mentioned ask
Topic, the following technical solution is employed by the present invention.
One aspect of the present invention is related to a kind of rosin acid sodium microemulsion, is made of following component and its weight percentage:
Rosin acid sodium 5-20%
Surfactant 2-20%
Solvent 2-10%
Cosolvent 2-10%
Defoaming agent 0.1-5%
Antifreezing agent 0.1-5%
Water supplies 100%.
Preferably, each component and its weight percentage are as follows:
Rosin acid sodium 8-15%
Surfactant 7-18%
Solvent 3-8%
Cosolvent 3-6%
Defoaming agent 0.5-2%
Antifreezing agent 03-4%
Water supplies 100%.
It is highly preferred that each component and its weight percentage are as follows:
Rosin acid sodium 10-12%
Surfactant 9-14%
Solvent 5-7%
Cosolvent 4-5%
Defoaming agent 0.5-1%
Antifreezing agent 2-4%
Water supplies 100%.
In formula of the present invention, wherein
The surfactant is selected from NONIN HS 240, tributyl phenyl polyglycol ether, polyoxyethylene mountain
One of pears alcohol fatty acid ester, dioctyl sodium sulphosuccinate, ethoxylated dodecyl alcohol sodium acetate are a variety of.
Preferably, the surfactant is selected from tributyl phenyl polyglycol ether, ethoxylated dodecyl alcohol sodium acetate
One or both of.
It is highly preferred that the surfactant is tributyl phenyl polyglycol ether and ethoxylated dodecyl alcohol 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。
The solvent is selected from acetone, toluene, chloroform, dimethylformamide, hexamethylene, Propylene Glycol ether, diformazan
One of base sulfoxide, petroleum ether are a variety of.Preferably one of acetone, dimethylformamide, dimethyl sulfoxide or a variety of.
The cosolvent is selected from one of ethyl alcohol, isopropanol, n-butanol, isobutanol, isoamyl alcohol or a variety of.It is preferably different
One of propyl alcohol, n-butanol, isoamyl alcohol are a variety of.
The defoaming agent is selected from n-octyl alcohol, dimethyl silicone polymer, polypropylene glycerol aether, butylphosphoric acid ester, phosphoric acid isobutyl
One of ester, silicone are a variety of.
The antifreezing agent is selected from one of ethylene glycol, glycerine, propylene glycol, polyethylene glycol or sorbierite or a variety of.
Another aspect of the present invention is related to the preparation method of the rosin acid sodium microemulsion, mainly comprises the following steps,
(1) solvent and cosolvent are uniformly mixed, rosin acid sodium are added later, and stir evenly, obtain oily phase；Wherein stir
Mixing speed can be 100-1000 revs/min, and mixing time is 30-60 minutes；
(2) surfactant, defoaming agent, antifreezing agent are added to the water, and stirred evenly, obtain water phase；Wherein stirring speed
Degree can be 100-1000 revs/min, and mixing time is 15-30 minutes；
(3) oil that step (1) obtains is added in the water phase that step (2) obtains while stirring, continues to stir, stirring speed
Degree can be 100-1000 revs/min, and mixing time is 15-40 minutes, and microemulsion is made.
The rosin acid sodium microemulsion stability that the present invention obtains is good, and every quality index is excellent, and insecticidal effect significantly improves.
Specific embodiment
In order to understand the present invention, the present invention is further illustrated with embodiment below, but do not limit the present invention.
(1) example of formulations
In following example of formulations, unless otherwise stated, the percentage is 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%.
Solvent and cosolvent are uniformly mixed, rosin acid sodium is added later, is stirred 40 minutes, is obtained with 200 revs/min of revolving speed
To oily phase.Surfactant, defoaming agent, antifreezing agent are added to the water, is stirred 25 minutes with 300 revs/min of revolving speed, obtains water
Phase.During the oil phase is added to the aqueous phase while stirring, stirring 30 minutes is continued with 300 revs/min of revolving speed, microemulsion is made.
Embodiment 2
Rosin acid sodium 15%, ethoxylated dodecyl alcohol sodium acetate 18%, dimethyl sulfoxide 8%, n-butanol 6%, polyoxy
Propylene glycerin ether 1%, propylene glycol 4%, water supplies 100%.
Solvent and cosolvent are uniformly mixed, rosin acid sodium is added later, is stirred 40 minutes, is obtained with 200 revs/min of revolving speed
To oily phase.Surfactant, defoaming agent, antifreezing agent are added to the water, is stirred 25 minutes with 300 revs/min of revolving speed, obtains water
Phase.During the oil phase is added to the aqueous phase while stirring, stirring 30 minutes is continued with 300 revs/min of revolving speed, microemulsion is made.
Embodiment 3
Rosin acid sodium 12%, tributyl phenyl polyglycol ether 8%, ethoxylated dodecyl alcohol sodium acetate 4%, dimethyl
Sulfoxide 6%, isopropanol 5%, phosphoric acid isobutyl ester 1%, polyethylene glycol 4%, water supplies 100%.
Solvent and cosolvent are uniformly mixed, rosin acid sodium is added later, is stirred 40 minutes, is obtained with 200 revs/min of revolving speed
To oily phase.Surfactant, defoaming agent, antifreezing agent are added to the water, is stirred 25 minutes with 300 revs/min of revolving speed, obtains water
Phase.During the oil phase is added to the aqueous phase while stirring, stirring 30 minutes is continued with 300 revs/min of revolving speed, microemulsion is made.
Embodiment 4
Rosin acid sodium 6%, tributyl phenyl polyglycol ether 2%, ethoxylated dodecyl alcohol sodium acetate 6%, acetone
4%, isopropanol 3%, silicone 0.5%, glycerine 2%, water supplies 100%.
Solvent and cosolvent are uniformly mixed, rosin acid sodium is added later, is stirred 40 minutes, is obtained with 200 revs/min of revolving speed
To oily phase.Surfactant, defoaming agent, antifreezing agent are added to the water, is stirred 25 minutes with 300 revs/min of revolving speed, obtains water
Phase.During the oil phase is added to the aqueous phase while stirring, stirring 30 minutes is continued with 300 revs/min of revolving speed, microemulsion is made.
Comparative example 1
Rosin acid sodium 12%, fatty alcohol polyoxyethylene ether 8%, calcium dodecyl benzene sulfonate 4%, dimethyl sulfoxide 6% are different
Propyl alcohol 5%, phosphoric acid isobutyl ester 1%, polyethylene glycol 4%, water supplies 100%.
Solvent and cosolvent are uniformly mixed, rosin acid sodium is added later, is stirred 40 minutes, is obtained with 200 revs/min of revolving speed
To oily phase.Surfactant, defoaming agent, antifreezing agent are added to the water, is stirred 25 minutes with 300 revs/min of revolving speed, obtains water
Phase.During the oil phase is added to the aqueous phase while stirring, stirring 30 minutes is continued with 300 revs/min of revolving speed, microemulsion is made.
Comparative example 2
Rosin acid sodium 8%, sodium lignin sulfonate 11%, dimethylformamide 5%, isopropanol 4%, dimethyl silicone polymer
0.5%, ethylene glycol 3%, water supplies 100%.
Solvent and cosolvent are uniformly mixed, rosin acid sodium is added later, is stirred 40 minutes, is obtained with 200 revs/min of revolving speed
To oily phase.Surfactant, defoaming agent, antifreezing agent are added to the water, is stirred 25 minutes with 300 revs/min of revolving speed, obtains water
Phase.During the oil phase is added to the aqueous phase while stirring, stirring 30 minutes is continued with 300 revs/min of revolving speed, microemulsion is made.
(2) determination of quality index
1, low-temperature stability measures
It is measured according to low-temperature stability of the GB-T 19137-2003 to invention formulation.Specially by sample at 0 DEG C
After storage 14 days, its cosmetic variation is observed.As a result it see the table below.
The measurement of 1 low-temperature stability of table
| Sample | As a result |
| Embodiment 1 | Substantially unchanged |
| Embodiment 2 | Substantially unchanged |
| Embodiment 3 | It is unchanged |
| Embodiment 4 | It is unchanged |
| Comparative example 1 | Lotion is muddy, there is lamination |
| Comparative example 2 | Lotion is muddy, there is lamination |
The results show that sample of the present invention is after cold storage, appearance is substantially unchanged.And then lotion is muddy for control sample, has
Lamination.
2, heat storage stability measures
It is measured according to heat storage stability of the GB-T 19136-2003 to invention formulation.Specially sample is placed in
In ampere bottle, after 54 DEG C are stored 14 days, observes appearance and simultaneously measure active component content, calculate resolution ratio.As a result it see the table below.
The measurement of 2 heat storage stability of table
| Sample | Appearance | Resolution ratio |
| Embodiment 1 | Substantially unchanged | 2.7% |
| Embodiment 2 | Substantially unchanged | 2.5% |
| Embodiment 3 | It is unchanged | 0.8% |
| Embodiment 4 | It is unchanged | 1.1% |
| Comparative example 1 | Layering | 9.5% |
| Comparative example 2 | Layering | 8.4% |
The results show that sample appearance of the present invention is substantially unchanged, and resolution ratio is lower, especially implements after overheat storage
Example 3-4 sample, almost without decomposition.In contrast, control sample is layered, and active ingredient breaks down rate is higher.
3, stability of emulsion measures
It is measured according to stability of emulsion of the GB/T 1603-2001 to invention formulation.Specifically, in 250ml beaker
In, 30 DEG C of 100ml of standard hard water is added, draws 1ml microemulsion sample with pipette, moves into graduated cylinder after mixing evenly, and
Graduated cylinder is placed in 30 DEG C of waters bath with thermostatic control, stands 1 hour, observation lotion separates situation.As a result as follows.
The measurement of 3 stability of emulsion of table
| Sample | As a result |
| Embodiment 1 | On without oil slick, lower no precipitating, clear |
| Embodiment 2 | On without oil slick, lower no precipitating, clear |
| Embodiment 3 | On without oil slick, lower no precipitating, clear |
| Embodiment 4 | On without oil slick, lower no precipitating, clear |
| Comparative example 1 | On have an oil slick, lotion is muddy |
| Comparative example 2 | On have an oil slick, lotion is muddy |
The results show that without oil slick, lower no precipitating, clear in lotion after sample of the present invention 1 hour.And control sample
Oil slick then is generated on lotion surface, lotion is muddy.
(3) field control effectiveness test
Invention formulation is tested to the control efficiency of cotton aphid.
Select aphid that consistent cotton plot occurs, division of cells, insect population is investigated before carrying out medicine.Only spray respectively
The medicament of 1-4 of the embodiment of the present invention and comparative example 1-2.Each processing dosage is consistent, controls as 25 active constituents/mu, every processing 3
Secondary repetition.Fresh water spraying is control.5 days investigation results after medicine calculate preventive effect.As a result it see the table below
The measurement of 4 field efficacy of table
| 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 control | - |
The results show that invention formulation significantly improves the preventive effect of cotton aphid relative to control formulation.
Examples detailed above is only that of the invention is explained further, and is not limitation of the invention, by by above-mentioned side
Case progress simply adjusts the scheme obtained from, equally within the scope of protection of this application.
Claims (2)
1. a kind of rosin acid sodium microemulsion, is made of following component and its weight percentage:
Rosin acid sodium 12%, tributyl phenyl polyglycol ether 8%, ethoxylated dodecyl alcohol sodium acetate 4%, dimethyl sulfoxide
6%, isopropanol 5%, phosphoric acid isobutyl ester 1%, polyethylene glycol 4%, water supplies 100%.
2. the preparation method of microemulsion according to claim 1, which is characterized in that comprise the following steps:
Solvent and cosolvent are uniformly mixed, rosin acid sodium is added later, is stirred 40 minutes with 200 revs/min of revolving speed, obtains oil
Phase；Surfactant, defoaming agent, antifreezing agent are added to the water, is stirred 25 minutes with 300 revs/min of revolving speed, obtains water phase；Side
Side is stirred during the oil phase is added to the aqueous phase, stirring 30 minutes is continued with 300 revs/min of revolving speed, microemulsion is made.
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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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| Publication number | Priority date | Publication date | Assignee | Title |
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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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| "农药微乳剂型的研究进展";王军 等;《河南农业科学》;20051231(第6期);第11页表1、第13页 |
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Effective date of registration: 20191204 Address after: 210000 No. 19 Zhaofeng Road, Changlu Street, Jiangbei New District, Nanjing City, Jiangsu Province Patentee after: Jiangsu Province Nongken Biological Chemical Co. Ltd. Address before: 210007 No. 5 Guanghua East Street, Jiangsu, Nanjing Patentee before: Gu Aiguo |