CN1989807A - Spinosad aqueous emulsion - Google Patents
Spinosad aqueous emulsion Download PDFInfo
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- CN1989807A CN1989807A CN 200510132526 CN200510132526A CN1989807A CN 1989807 A CN1989807 A CN 1989807A CN 200510132526 CN200510132526 CN 200510132526 CN 200510132526 A CN200510132526 A CN 200510132526A CN 1989807 A CN1989807 A CN 1989807A
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- aqueous emulsion
- multiple killing
- killing teichomycin
- water
- ether
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Abstract
The invention provides a method which products plant source broad-spectrum fusidic acid aqueous emulsion using technique of double crossing, it increases the efficacy of broad-spectrum fusidic acid aqueous emulsion and reduces the use of organic solvents in the largest degree, thereby reduces environmental pollution of pesticide, improves utilization ratio and safety of product; meanwhile, it increases stability of pharmaceuticals storage and the adhesiveness and penetrability to plant of pharmaceuticals, so the effect of anti-pest is high and the period is long.The aqueous emulsion of the invention is prepared by broad-spectrum fusidic acid, assisting solvent, stabilizer, emulsifier and water. The synergism of the invention is significant, and the invention increases the safety when using.
Description
Technical field
The invention belongs to the pesticide producing field, be specially a kind of type agent of botanical pesticide spinosad aqueous emulsion and production method thereof of containing.
Background technology
Along with being extensive use of of chemical pesticide, how to reduce the pollution of environment and, more and more paid close attention to by people to people and animals' murder by poisoning, therefore, reduce toxicity, the raising drug effect is the inexorable trend that agricultural chemicals develops.Researching and developing the purpose that realizes reducing toxicity, improves drug effect by formulation is a kind of comparatively economy mode efficiently for former medicine research and development.At present, China is relatively backward aspect formulations of pesticide research and development, and basically based on missible oil and wetting powder, its consumption accounts for the 70-80% of total amount of formulation; And formulation is more single, and the ratio of former medicine and preparation is 1: 6, then about 1: 30 of developed country, and both fall far short.Obviously, this can not adapt to current agricultural production development, especially agricultural product structural adjustment far away to the variation of agricultural chemicals demand, and can influence the marketing and the service life of Pesticidal products to a great extent.Simultaneously, the single operation technique that also can cause of the formulations of pesticide falls behind.Pay attention to the transformation of existing formulation, develop the novel form that meets production and environmental requirement, not only adapt to the requirement of sustainable development, also can remedy the deficiency of former medicine development ability simultaneously.
In numerous formulations of pesticide, comparatively convenient and general use is a liquid formulation, and wherein using maximum formulations for a long time is missible oil.Missible oil needs to use a large amount of organic solvents in process, as benzene,toluene,xylene or the like, the use of a large amount of organic solvents not only causes the waste of industrial chemicals, and since the combustibility of solvent on transportation, storage and container selection, also be restricted.Simultaneously, brought very big murder by poisoning for environment and human health, with the economic development and the environment for human survival of entail dangers to country.Developed country limits or forbids using in a large number the pesticide new variety registration of toxic organic solvent preparations such as benzene,toluene,xylene from sustainable development target.Therefore, develop novel liquid formulation, become the trend of the times of agricultural chemicals development to reduce or eliminate these virulent organic solvents.Wherein, Water-borne modification is exactly one of dominant direction of formulations of pesticide development.And, the novel form of agricultural chemicals also can increase new feature to agricultural chemicals, more can give full play to the action characteristic of former medicine self, overcome and remedy the deficiency of the original formulation of agricultural chemicals, toxicity and excitant to people and animals are all lower, and can alleviate the poisoning to crop, improve physico chemistry and biological property, enlarge range of application, prolong the service life of medicament etc.
Aqueous emulsion (Emulsion in water) is one of novel form that meets the agricultural chemicals developing direction, international code name: the EW of formulation, be the water-fast solution of former medicine of water-fast liquid state or solid-state former drug solns organic solvent gained, be scattered in the water, form a kind of environmentally friendly type pesticidal preparations, the active component drop disperses the back particle diameter less than 2 microns, and outward appearance is an opaque and white emulsion, and it is a kind of oil-water type (O/W) emulsion.Strong to plant and insect tissue cell permeability, the absorption ratio height, preventive effect is good, simultaneously, has production, storing and safe in utilization, and environmental pollution is little, helps the improvement of ecotope.
In the eighties in last century, external existing aqueous emulsion data and the patent report developed, have part aqueous emulsion commodity the beginning of the nineties, is a kind of pesticides new formulation.About the water and milkization of botanical pesticide multiple killing teichomycin (spinosad), the dish happiness
2.5% suspending agent is the up-to-date insecticide of developing successfully of new generation of The Dow Agrosciences, LLC., at present successfully listing.But yet there are no the research report of spinosad aqueous emulsion so far.
Summary of the invention
The purpose of this invention is to provide a kind of spinosad aqueous emulsion and production method thereof, particular content is as follows:
Spinosad aqueous emulsion of the present invention is made up of the former medicine of multiple killing teichomycin, cosolvent, emulsifier, stabilizing agent and water, and wherein the percentage by weight of various components is:
Multiple killing teichomycin 1～10%
Cosolvent 1～10%
Emulsifier 5～20%
Stabilizing agent 1～5%
Water 55～92%
Wherein the stabilizing agent preferred amounts is 1～3%.
Among the present invention, cosolvent is meant alcohols (as ethanol, isopropyl alcohol, n-butanol, n-amyl alcohol, hexanol etc.), ketone (as acetone, cyclohexanone etc.), amide-type (as dimethyl formamide etc.), naphthenic (as cyclohexane etc.), aromatic hydrocarbons (as benzene,toluene,xylene, Fluhyzon etc.), also can be to well known to a person skilled in the art other cosolvent.Cosolvent can be any one or two or more combination wherein.Preferred cosolvent is selected from ethanol, isopropyl alcohol, n-butanol, n-amyl alcohol, acetone, cyclohexanone, dimethyl formamide, cyclohexane, benzene, toluene and dimethylbenzene.
Among the present invention, emulsifier is meant non-ionic surface active agent and/or anion surfactant.The non-ionic surface active agent that can adopt is for example castor oil ethylene oxide adduct, phenethyl phenol polyethenoxy ether, phenethyl phenol polyethenoxy polyethenoxy ether, phenethyl phenol polyethenoxy ether phosphate, alkylphenol polyoxyethylene formaldehyde condensation products, benzylbiphenyl phenol polyethenoxy ether, alkylphenol polyoxyethylene, xenol APEO etc.The anion surfactant that can adopt be for example alkylbenzenesulfonate (as C
10-C
14-alkyl benzene calcium sulfonate, magnesium, sodium salt), C
8-C
20-alkylsurfuric acid sodium salt (as lauryl sodium sulfate salt), styrene polyoxyethylene ether ammonium sulfate salt etc.Preferably, the compound of non-ionic surface active agent and anion surfactant.When the present invention specifically implements, preferably adopt commercially available various emulsifier types, for example, emulsifier can be selected from No. 500, farming breast, agricultural emulsifier NO series (as the newborn 601-606 of farming number), Nongru-700 series is (as peaceful newborn No. 36, No. 37, peaceful breast, Nongru-700-1,700-2, the newborn SPF of farming), NP-10, No. 1600 series of farming breast are (as farming breast 1601,1602, peaceful breast 33, No. 34), No. 2000, farming breast, No. 11, farming breast, No. 12, farming breast, PF-690, BY series is (as peaceful newborn 110,120,130,140, the EL emulsifier), tween series is (as Tween-40, Tween-60, Tween-80), Sorpol series (Sorpol KS, Sorpol KD, Sorpol-2676, Sorpol-2678S etc.) or have any one or two or more combinations in the emulsifier of similar features.
Can also contain stabilizing agent in case of necessity in the pesticide emulsion in water of the present invention, be used to increase the physics and the chemical stability of aqueous emulsion.Accord with stabilizing agent of the present invention and be for example 2-expoxy propane, butyl glycidyl ether, polyethylene glycol diglycidyl ether or sorbierite, isopropyl alcohol, n-butanol, ethylene glycol, polyethylene glycol, urea, propane diols, glycerine, turpentine oil and well known to a person skilled in the art in the stabilizing agent any one.Preferably ethylene glycol, polyethylene glycol, glycerine, turpentine oil and urea, this class stabilizing agent has the dual function of stabilizing agent and antifreezing agent.Its consumption is 1-10%.
The water that adopts among the present invention can be running water, deionized water etc., preferably deionized water such as distilled water.
The present invention also comprises the preparation method of pesticide emulsion in water of the present invention, these method process following steps,
A. former medicine of multiple killing teichomycin and cosolvent are mixed;
B. add emulsifier, stabilizing agent, water;
C. mix.
Below be one of adoptable method:
The former medicine of multiple killing teichomycin is dissolved in the cosolvent, drops into emulsifier, stir (can suitably heat), put into then and mix strongly in the homogenizer that dispersion medium water is housed and homogenize, promptly get spinosad aqueous emulsion.
Also can adopt following method:
The former medicine of multiple killing teichomycin is dissolved in the cosolvent, drops into emulsifier, drop into stabilizing agent again, stir (can suitably heat), put into then and mix strongly in the homogenizer that dispersion medium water is housed and homogenize, promptly get spinosad aqueous emulsion.
The technology of the present invention advance is with water to be matrix, and with the system that two phases (particularly O/W type) exist, active ingredient is distributed between the 100-700nm.Show following characteristics: synergistic effect is remarkable, Environmental compatibility good, activity is high, safety is good, production cost is low, market capacity is big.
Adopt pesticide emulsion in water of the present invention can farthest reduce the use of organic solvent, and synergistic effect is remarkable, thereby reduces the pollution of agricultural chemicals, improve safety in utilization environment; Simultaneously, because the processing characteristics of preparation of the present invention has also improved the medicament storage-stable, and to adhesiveness and the permeability of plant, to insect preventive effect height, the lasting period is long.
Adopt not limited embodiment to be enumerated explanation hereinafter.
Embodiment
Pesticide emulsion in water of the present invention adopts following method preparation:
Embodiment 1: 28 kilograms of the multiple killing teichomycins with 90% and 10 kilograms of ethanol mix, and suitably heating for dissolving drops into 110 kilograms of farming breasts 500 again
#With 1602
#, and 10 kilograms of ethylene glycol stabilizing agents and stirring, drop into then and be equipped with in 842 kilograms of dispersion medium water, give homogenizer and be mixed to strongly evenly.Promptly get 1000 kilogram of 2.5% spinosad aqueous emulsion.
Its middle peasant's breast 500
#, 1602
#For: the code name of alkyl benzene calcium sulfonate, phenethyl phenol polyethenoxy polyethenoxy ether material, buy certainly: chemical plant, Lvshun, Dalian
Embodiment 2: spinosad aqueous emulsion the key technical indexes of the present invention is as shown in table 1
The quality of the above-mentioned aqueous emulsion product that table 1 is prepared meets following technical indicator after tested:
| Index name | Index |
| Multiple killing teichomycin content (%m/m) (20 ℃) | ≥2.5 |
| PH value | 5.0-7.0 |
| Stability of emulsion (diluting 200 times) | Qualified |
| Low-temperature stability (0 ± 2 ℃) | Qualified |
| Heat storage stability (54 ± 2 ℃) | ≤4 |
| Pourability | Qualified |
| Annotate: low-temperature stability and heat storage stability test, carried out once at least in per 3 months | |
EXPERIMENTAL EXAMPLE 3:2.5% spinosad aqueous emulsion is to the Toxicity Determination experiment of diamond-back moth
Present embodiment is the Toxicity Determination experiment of carrying out at diamond-back moth, and the antagonism diamond-back moth has virulence preferably, and measurement result is as shown in table 2:.
Reagent agent:
1,2.5% dish happiness
Suspending agent (commercially available prod, the Dow Chemical Company produces);
2,2.5% spinosad aqueous emulsion (example of formulations 1 of the present invention);
Experiment is a diamond-back moth with worm, and 3 instar larvaes are tested by Institute of Vegetables, Chinese Academy of Agricultural Sciences.
The employing leaf dipping method is measured, and measures the virulence of tagging of above-mentioned medicament.Drug concentration adopts 6 concentration gradients to handle, and every processing repeats for 6 times, 48 of every duplication examination worms.Put into constant incubator cultivation investigation in 48 hours insect population lethality and see the following form 2.
Table 2 spinosad aqueous emulsion is to the Toxicity Determination result of cotton bollworm
| Reagent agent | Review time | Toxicity regression formula (Y=) | LC 50(95% confidence limit) (μ g/ml) | LC 90Value (μ g/ml) | The synergy multiple |
| Medicament 2 | 48h | Y＝-2.50+2.70X(±0.3782) | 8.4212 | 73.0692 | 2.96 |
| Medicament 1 | Y＝-2.48+2.76X(±0.3645) | 2.8457 | 18.3532 | 1.00 |
Annotate: the LC of synergy multiple=contrast medicament
50The LC of value/synergy medicament
50Value
EXPERIMENTAL EXAMPLE 4:30% spinosad aqueous emulsion is tested the cotton bollworm control field efficacy
Present embodiment is the field efficacy experiment of carrying out at diamond-back moth.
Experimental condition: experimental field be Hebei experiment wild cabbage ground, the experiment kind be in sweet No. 17, the seeding method program request, density 30cm * 30cm, rich water quality management unanimity in the experiment sub-district, the growing way unanimity, it is medium that worm is measured generation.Worm age is mostly in 3 ages.
Reagent agent:
1,2.5% dish happiness
Suspending agent (multiple killing teichomycin commercially available prod, the Dow Chemical Company produces);
2,2.5% spinosad aqueous emulsion (example of formulations 1 of the present invention);
Spray method: above-mentioned five processing, each repeats twice, 15 square metres of each sub-district areas, the experimental plot is district's group arrangement at random in the field.With the conventional spraying of KIM-9MATABI knapsack hand sprayer.
Investigation method: take five point samplings in each sub-district before the spray medicine, all borer populations of living of fixed point investigation 5-10 strain, as the insect population radix, 1,7 day remaining borer population alive of investigation behind the medicine.
Result of the test shows that the control efficiency of 2 pairs of diamond-back moths of medicament obviously improves than medicament 1, significance test, and control efficiency increases significantly.The result sees following table for details.
The field efficacy experimental result of table 3 spinosad aqueous emulsion control cotton bollworm
| Reagent agent and concentration | Repeat | Worm lives before the medicine | Behind the medicine 1 day | Behind the medicine 7 days | ||||
| Borer population alive | Rate goes down | Correcting controling effect | Borer population alive | Rate goes down | Correcting controling effect | |||
| Medicament 1 1500X | 1 | 50 | 14 | 72 | 72b | 9 | 82 | 81b |
| 2 | 51 | 14 | 72 | 10 | 80 | |||
| Medicament 2 1500X | 1 | 50 | 7 | 84 | 84a | 2 | 96 | 96a |
| 2 | 51 | 8 | 84 | 2 | 96 | |||
| CK | 1 | 30 | 30 | 0 | 30 | 0 | ||
| 2 | 31 | 31 | 0 | 30 | 3.2 | |||
Test period :-11 days on the 4th July in 2005, numeral back, table back English alphabet difference, the expression significant difference (p=0.05, HSD)
Poisoning does not take place in for examination concentration.Field experiment shows, aqueous emulsion of the present invention is compared with similar medicament the diamond-back moth control efficiency in the field has significant difference.
Embodiment 5: the particle size distribution range of the spinosad aqueous emulsion of preparing with the embodiment of the invention 1, result such as following table 4.
The above-mentioned aqueous emulsion product that adopts the embodiment of the invention 1 to prepare, particle size distribution range are measured and are adopted transmission electron microscope (TEM) and laser particle size analysis method, and the present invention is carried out grain size analysis, and analysis result is as follows:
The performance of the spinosad aqueous emulsion that table 4 is prepared with the embodiment of the invention 1
| Method name | Granularity (nm) |
| Transmission electron microscope | 500 |
| Laser particle size analysis | 100～700 |
Though above the present invention is described in detail with a general description of the specific embodiments, on basis of the present invention, can make some modifications or improvements it, this will be apparent to those skilled in the art.Therefore, not departing from the these modifications or improvements basically of spirit of the present invention, all belong to the scope of protection of present invention.
Claims (6)
1, a kind of aqueous emulsion that contains the botanical pesticide multiple killing teichomycin wherein contains multiple killing teichomycin, surfactant, cosolvent, stabilizing agent, water, it is characterized in that:
(a) weight percentage is 1～10% multiple killing teichomycin;
(b) surfactants/cosurfactants is castor oil ethylene oxide adduct, phenethyl phenol polyethenoxy ether, phenethyl phenol polyethenoxy polyethenoxy ether, phenethyl phenol polyethenoxy ether phosphate, alkylphenol polyoxyethylene formaldehyde condensation products, benzylbiphenyl phenol polyethenoxy ether, alkylphenol polyoxyethylene, xenol APEO, alkylbenzenesulfonate, C
8-C
20Some or certain mixture of two in-alkylsurfuric acid sodium salt, the styrene polyoxyethylene ether ammonium sulfate salt, weight percentage is 5～20%;
(c) cosolvent is ethanol, isopropyl alcohol, n-butanol, n-amyl alcohol, hexanol, acetone, cyclohexanone, dimethyl formamide, cyclohexane, benzene,toluene,xylene, Fluhyzon, and weight percentage is 1～10%;
(d) stabilizing agent is 2-expoxy propane, butyl glycidyl ether, polyethylene glycol diglycidyl ether, sorbierite, isopropyl alcohol, n-butanol, ethylene glycol, polyethylene glycol, urea, propane diols, glycerine, turpentine oil, and weight percentage is 1～5%; Surplus is water or deionized water.
2, a kind of aqueous emulsion that contains the botanical pesticide multiple killing teichomycin according to claim 1, wherein surfactants/cosurfactants is alkylbenzenesulfonate and phenethyl phenol polyethenoxy polyethenoxy ether.
3, a kind of aqueous emulsion that contains the botanical pesticide multiple killing teichomycin according to claim 1, wherein stabilizing agent is an ethylene glycol.
4, a kind of method for producing aqueous emulsion that contains the botanical pesticide multiple killing teichomycin according to claim 1, it is characterized in that at first the ethanol that accounts for preparation preparation total amount 1～10%, adding being accounted in the multiple killing teichomycin of preparation preparation total amount 1～10%, can suitably heat, be stirred well to fully evenly, add 5～20% surfactants/cosurfactants and 1～5% stabilizing agent then and mix; Under stirring condition, add in required water or the deionized water then, be stirred to homogeneous phase, outward appearance is working fluid, leaves standstill, filters, and promptly gets 1～10% spinosad aqueous emulsion.
5, the preparation method of spinosad aqueous emulsion according to claim 4 is characterized in that the present invention can be used for producing binary or the ternary built aqueous emulsion or the suspending agent of multiple killing teichomycin and other insecticide, bactericide, weed killer herbicide and plant growth regulator.
6, a kind of aqueous emulsion that contains the botanical pesticide multiple killing teichomycin is preparing according to the application in arbitrary pesticide emulsion in water of claim 1-5.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200510132526 CN1989807A (en) | 2005-12-26 | 2005-12-26 | Spinosad aqueous emulsion |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200510132526 CN1989807A (en) | 2005-12-26 | 2005-12-26 | Spinosad aqueous emulsion |
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| Publication Number | Publication Date |
|---|---|
| CN1989807A true CN1989807A (en) | 2007-07-04 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101889571A (en) * | 2010-07-08 | 2010-11-24 | 河北益海安格诺农化有限公司 | Spinosad soluble agent and preparation method thereof |
| CN101720766B (en) * | 2009-12-29 | 2012-08-22 | 华南农业大学 | Insecticidal composition of tea saponin and pleocidin |
| CN106305764A (en) * | 2016-08-20 | 2017-01-11 | 广东中迅农科股份有限公司 | Environment-friendly emulsion-in-water compounded by flusilazole and prochloraz and preparation method of environment-friendly emulsion-in-water |
| CN111567530A (en) * | 2020-07-06 | 2020-08-25 | 济南中科绿色生物工程有限公司 | Spinosad insecticide and application thereof |
-
2005
- 2005-12-26 CN CN 200510132526 patent/CN1989807A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101720766B (en) * | 2009-12-29 | 2012-08-22 | 华南农业大学 | Insecticidal composition of tea saponin and pleocidin |
| CN101889571A (en) * | 2010-07-08 | 2010-11-24 | 河北益海安格诺农化有限公司 | Spinosad soluble agent and preparation method thereof |
| CN101889571B (en) * | 2010-07-08 | 2013-02-13 | 河北益海安格诺农化有限公司 | Spinosad soluble agent and preparation method thereof |
| CN106305764A (en) * | 2016-08-20 | 2017-01-11 | 广东中迅农科股份有限公司 | Environment-friendly emulsion-in-water compounded by flusilazole and prochloraz and preparation method of environment-friendly emulsion-in-water |
| CN111567530A (en) * | 2020-07-06 | 2020-08-25 | 济南中科绿色生物工程有限公司 | Spinosad insecticide and application thereof |
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