CN102599160B - Flubendiamide and Spinetoram compound suspending agent and preparation method thereof - Google Patents
Flubendiamide and Spinetoram compound suspending agent and preparation method thereof Download PDFInfo
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- CN102599160B CN102599160B CN201210019260.4A CN201210019260A CN102599160B CN 102599160 B CN102599160 B CN 102599160B CN 201210019260 A CN201210019260 A CN 201210019260A CN 102599160 B CN102599160 B CN 102599160B
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Abstract
The invention discloses a flubendiamide and Spinetoram compound suspending agent and a preparation method of the compound suspending agent. The compound suspending agent comprises the following raw material components in percentage by weight: 0.2-38% of flubendiamide, 0.5-12% of Spinetoram, 0.5-6% of dispersant, 0.5-5% of wetting agent, 0.1-4.5% of thickening agent, 2-8% of antifreezing agent, 0.1-0.8% of preservative, 0.1-0.6% of defoaming agent and 36.0-88.0% of water. The preparation method comprises the steps of: mixing and shearing flubendiamide, Spinetoram, the dispersant, the wetting agent, the thickening agent, the antifreezing agent, the preservative, the defoaming agent and water for uniformly dispersing, then sanding and screening. According to the invention, the compound suspending agent is wide in pest control spectrum, and the pesticide resistance is difficult for pests to generate; the preparing process is simpler and the production cost is lower; and a great deal of organic solvent is not needed, so that the cost is lowered, and the stimulation to operators and pollution to environment of the organic solvent are reduced.
Description
Technical field
The invention belongs to technical field of pesticide, relate to a kind of agriculture chemical compounding insecticide, be specifically related to fipronil bisamide and the composite suspending agent of ethyl pleocidin and preparation method thereof.
Background technology
In chemical pesticide, contain a large amount of organic solvents, when making huge contribution for agricultural foison, also to natural environment, brought serious pollution.Along with environmental regulation becomes better and approaching perfection day by day, the cry that reduces pesticide pollution is day by day strong.Develop safely, environmental protection and cheap novel liquid formulation have become the trend of the times of Agrochemicals to reduce or eliminate organic solvent harm.Wherein, Water-borne modification is exactly one of dominant direction of formulations of pesticide development.This class pesticides new formulation also can increase new feature to agricultural chemicals, more can give full play to the function Characteristics of former medicine self, overcome and make up the deficiency of the original formulation of agricultural chemicals, all lower to people and animals' toxicity and excitant, and can alleviate the poisoning to crop, improve physico chemistry and biological property, expand range of application, extend the service life of medicament.
Agricultural chemicals suspension agent belongs to one of Water-borne modification novel form, is pesticide active ingredient and dispersant, wetting agent, thickener, defoamer, antifreezing agent etc. to be dispersed in matrix water and the high dispersive forming, stable suspended substance.Agricultural chemicals suspension agent has the advantage of wetting powder and missible oil concurrently: aspect drug effect, suspending agent herbicide effects is better than wetting powder, and insecticide effect is close with missible oil; Because agricultural chemicals suspension agent be take water as dispersion medium, make it have environmental protection, cheap feature, reduced the use of a large amount of organic solvents simultaneously, production process is safe, pollution-free; And suspending agent can mix with arbitrary proportion with water, easy to use, after dilution, can reach larger coverage rate, can be processed to the formulation of high concentration.
Fipronil bisamide chemical name is the iodo-N ' of 3--(2-mesyl)-1,1-dimethyl ethyl group-N-{4-[1,2,2,2-tetrafluoro-1-(trifluoromethyl) ethyl]-O-tolyl } phthalic amide.Belong to Novel ortho benzenedicarboxamide insecticides, insect ryania (muscle) receptor activators, completely different from the mechanism of action of insecticide in the past, can make excessively to discharge calcium ion in insect bodies, cause insect death.This insecticide does not produce cross resistance with existing insecticide, and efficient, safety, is rising novel pesticide.
Ethyl pleocidin is comprised of ethyl pleocidin-J and two kinds of components of ethyl pleocidin-L, and ethyl pleocidin-J outward appearance is white powder, and ethyl pleocidin-L outward appearance is white to yellow crystals, band semen armeniacae amarae taste.Ethyl pleocidin acts on nAChR and r-aminobutyric acid acceptor in insect nerve, causes polypide insensitive to the signal transfer reaction of excitability or inhibition, affects normal nervous activity, until dead.Ethyl pleocidin has stomach toxicity and action of contace poison, is mainly used in preventing and treating diamond-back moth, beet armyworm, Liriomyza, prodenia litura and lima bean pod borer.
At present, there are no fipronil bisamide and ethyl pleocidin composite be the report of suspending agent.
Summary of the invention
The object of the invention is for the deficiencies in the prior art, provide a kind of wide to control of insect spectrum, insect is difficult to develop immunity to drugs, safety and environmental protection, the fipronil bisamide that environmental pollution is little and the composite suspending agent of ethyl pleocidin and preparation method thereof.Composite suspending agent preparation technology of the present invention is simple, production cost is lower.
Fipronil bisamide insecticidal action mechanism is different from ethyl pleocidin, and the two is composite for not only having expanded control of insect spectrum after suspending agent, and has increased the action target spot of medicament, can delay pest resistance to insecticide.
The suspending agent that water-fast solid pesticide is processed into itself is a kind of thermodynamic unstable system between colloid and rough segmentation system.The present invention, in the preparation process of suspending agent, is added with the auxiliary agents such as wetting agent, dispersant and antifreezing agent, and the Main Function of wetting agent and dispersant is: increase dispersion medium viscosity, reduce the difference in specific gravity between dispersion medium and disperse phase.Through auxiliary agent and active component, mutually coordinate, kept the stability of preparation.The prepared suspending agent of the present invention has that particle diameter is little, biologically active is high and the feature such as using dosage is low, and take water as medium, and it is environmentally friendly.
For reaching above object, the present invention has adopted following technical scheme:
The composite suspending agent of fipronil bisamide and ethyl pleocidin, by weight percentage, the raw material proportioning of described composite each component of suspending agent is: fipronil bisamide 0.2～38%, ethyl pleocidin 0.5～12%, dispersant 0.5～6%, wetting agent 0.5～5%, thickener 0.1～4.5%, antifreezing agent 2～8%, preservative 0.1～0.8%, defoamer 0.1～0.6%, water 36.0～88.0%;
Described dispersant is one or both in sodium lignin sulfonate, Negel and fatty alcohol-polyoxyethylene ether;
Described wetting agent is one or both in alkylsurfuric acid calcium, alkyl sulfonic acid calcium or phenethyl phenol polyethenoxy ether sodium sulfate;
Described thickener is bentonite or xanthans;
Described antifreezing agent is ethylene glycol or glycerine;
Described preservative is sodium salicylate or potassium sorbate;
Described defoamer is n-octyl alcohol.
Further, described water is preferably distilled water or deionized water.
The percentage by weight of described fipronil bisamide in raw material is preferably 5～25%, and the percentage by weight of ethyl pleocidin in raw material is preferably 5～10%.
The preparation method of described fipronil bisamide and the composite suspending agent of ethyl pleocidin, after fipronil bisamide, ethyl pleocidin, dispersant, wetting agent, thickener, antifreezing agent, preservative, defoamer and water being mixed by raw material proportioning, shear and be dispersed to evenly, through sand milling, it is fipronil bisamide and the composite suspending agent of ethyl pleocidin of 0.5～5 μ m that screening obtains particle diameter again.
Further, the rotating speed of described dispersion is preferably 1000～3000r/min, and the time is preferably 25～60min.
The rotating speed of described sand milling is preferably 1400～1600r/min, and the time is preferably 0.5～2.5h; It is to carry out in high-shearing dispersion emulsifying machine that described shearing disperses.
Compared with prior art, tool has the following advantages in the present invention:
(1) the composite suspending agent of the present invention is wide to control of insect spectrum, and insect is difficult to develop immunity to drugs;
(2) preparation technology of the composite suspending agent of the present invention is simpler, and production cost is lower;
(3) in the production process of the composite suspending agent of the present invention, do not use a large amount of organic solvents, safety and environmental protection, environmental pollution is little;
(4) the composite suspending agent of the present invention, not containing a large amount of organic solvents, meets the requirement of environmental type agricultural chemicals, is appropriate to the scale of chemical production.
Embodiment
Below in conjunction with embodiment, the invention will be further described, but the scope of protection of present invention is not limited to this.
Embodiment 1
Take fipronil bisamide 0.2kg, ethyl pleocidin 12.0kg, sodium lignin sulfonate 1.5kg, alkylsurfuric acid calcium 2.5kg, bentonite 1.2kg, ethylene glycol 4.8kg, sodium salicylate 0.65kg, n-octyl alcohol 0.35kg and distilled water 76.8kg in high-shearing dispersion emulsifying machine, under 3000r/min rotating speed, disperse 25min, the sand mill sand milling 2h that is 1500r/min through rotating speed again, it is that 0.5～5 μ m, content are 12.2% fipronil bisamide and the composite suspending agent of ethyl pleocidin that screening obtains particle diameter.According to pesticide field efficacy medicine test criterion, carry out dispenser and biologically active statistics, use 2000 times of liquid of said preparation to carry out field control effectiveness test, the control efficiency of the 6th day and 10 days after the medication of cotton cotton bollworm is respectively to 91.5% and 92.7%.
Embodiment 2
Take fipronil bisamide 38.0kg, ethyl pleocidin 0.5kg, Negel 3.2kg, alkyl sulfonic acid calcium 1.8kg, xanthans 1.5kg, glycerine 5.5kg, potassium sorbate 0.35kg, n-octyl alcohol 0.15kg and deionized water 49.0kg in high-shearing dispersion emulsifying machine, under 2500r/min rotating speed, disperse 35min, the sand mill sand milling 2.5h that is 1400r/min through rotating speed again, it is that 0.5～5 μ m, content are 38.5% fipronil bisamide and the composite suspending agent of ethyl pleocidin that screening obtains particle diameter.According to pesticide field efficacy medicine test criterion, carry out dispenser and biologically active statistics, use 4000 times of liquid of said preparation to carry out field control effectiveness test, the control efficiency of the 7th day and 12 days after the medication of wild cabbage prodenia litura is respectively to 92.5% and 94.3%.
Embodiment 3
Take fipronil bisamide 0.2kg, ethyl pleocidin 0.5kg, fatty alcohol-polyoxyethylene ether 0.6kg, phenethyl phenol polyethenoxy ether sodium sulfate 1.4kg, bentonite 3.0kg, ethylene glycol 5.3kg, sodium salicylate 0.45kg, n-octyl alcohol 0.55kg and distilled water 88.0kg in high-shear emulsion machine, under 2500r/min rotating speed, disperse 45min, the sand mill sand milling 2h that is 1500r/min through rotating speed again, it is that 0.5～5 μ m, content are 0.7% fipronil bisamide and the composite suspending agent of ethyl pleocidin that screening obtains particle diameter.According to pesticide field efficacy medicine test criterion, carry out dispenser and biologically active statistics, use 2000 times of liquid of said preparation to carry out field control effectiveness test, the control efficiency of the 5th day and 10 days after the medication of cotton cotton bollworm is respectively to 82.5% and 84.1%.
Embodiment 4
Take fipronil bisamide 38.0kg, ethyl pleocidin 12.0kg, sodium lignin sulfonate 1.6kg, Negel 1.0k, alkylsurfuric acid calcium 3.4kg, xanthans 2.5kg, glycerine 4.5kg, potassium sorbate 0.8kg, n-octyl alcohol 0.2kg and deionized water 36.0kg in high-shear emulsion machine, under 1000r/min rotating speed, disperse 60min, the sand mill sand milling 1.5h that is 1500r/min through rotating speed again, it is that 0.5～5 μ m, content are 50.0% fipronil bisamide and the composite suspending agent of ethyl pleocidin that screening obtains particle diameter.According to pesticide field efficacy medicine test criterion, carry out dispenser and biologically active statistics, use 5000 times of liquid of said preparation to carry out field control effectiveness test, control efficiency to the 6th day and 10 days after the medication of wild cabbage prodenia litura is respectively 92.6% and 94.5%, and the control efficiency of the 7th day and 14 days after the medication of cotton cotton bollworm is respectively to 93.2% and 95.9%.
Embodiment 5
Take fipronil bisamide 32.0kg, ethyl pleocidin 10.0kg, sodium lignin sulfonate 0.2kg, fatty alcohol-polyoxyethylene ether 0.3kg, alkyl sulfonic acid calcium 4.5kg, bentonite 2.0kg, ethylene glycol 2.0kg, sodium salicylate 0.1kg, n-octyl alcohol 0.6kg and distilled water 48.3kg in high-shear emulsion machine, under 2800r/min rotating speed, disperse 30min, the sand mill sand milling 1.5h that is 1600r/min through rotating speed again, it is that 0.5～5 μ m, content are 42.0% fipronil bisamide and the composite suspending agent of ethyl pleocidin that screening obtains particle diameter.According to pesticide field efficacy medicine test criterion, carry out dispenser and biologically active statistics, use 4500 times of liquid of said preparation to carry out field control effectiveness test, control efficiency to the 5th day and 10 days after the medication of beet prodenia litura is respectively 90.3% and 91.7%, and the control efficiency of the 6th day and 12 days after the medication of cotton cotton bollworm is respectively to 91.2% and 89.6%.
Embodiment 6
Take fipronil bisamide 26.0kg, ethyl pleocidin 8.0kg, Negel 1.5kg, fatty alcohol-polyoxyethylene ether 1.0kg, phenethyl phenol polyethenoxy ether sodium sulfate 0.5kg, xanthans 0.1kg, glycerine 3.5kg, potassium sorbate 0.55kg, n-octyl alcohol 0.45kg and deionized water 58.4kg in high-shear emulsion machine, under 2000r/min rotating speed, disperse 50min, the sand mill sand milling 1h that is 1500r/min through rotating speed again, it is that 0.5～5 μ m, content are 34.0% fipronil bisamide and the composite suspending agent of ethyl pleocidin that screening obtains particle diameter.According to pesticide field efficacy medicine test criterion, carry out dispenser and biologically active statistics, use 3500 times of liquid of said preparation to carry out field control effectiveness test, the control efficiency of the 6th day and 12 days after the medication of wild cabbage prodenia litura is respectively to 92.1% and 90.5%.
Embodiment 7
Take fipronil bisamide 20.0kg, ethyl pleocidin 6.0kg, sodium lignin sulfonate 1.8kg, alkylsurfuric acid calcium 1.0kg, alkyl sulfonic acid calcium 1.2kg, bentonite 2.6kg, ethylene glycol 6.4kg, sodium salicylate 0.2kg, n-octyl alcohol 0.4kg and distilled water 60.4kg in high-shear emulsion machine, under 3000r/min rotating speed, disperse 40min, the sand mill sand milling 0.5h that is 1600r/min through rotating speed again, it is that 0.5～5 μ m, content are 26.0% fipronil bisamide and the composite suspending agent of ethyl pleocidin that screening obtains particle diameter.According to pesticide field efficacy medicine test criterion, carry out dispenser and biologically active statistics, use 3000 times of liquid of said preparation to carry out field control effectiveness test, control efficiency to the 5th day and 8 days after the medication of wild cabbage prodenia litura is respectively 90.3% and 92.5%, and the control efficiency of the 6th day and 10 days after the medication of cotton cotton bollworm is respectively to 93.8% and 95.2%.
Embodiment 8
Take fipronil bisamide 15.0kg, ethyl pleocidin 5.0kg, Negel 4.4kg, alkylsurfuric acid calcium 2.5kg, phenethyl phenol polyethenoxy ether sodium sulfate 2.5kg, xanthans 3.5kg, glycerine 2.5kg, potassium sorbate 0.5kg, n-octyl alcohol 0.5kg and deionized water 63.6kg in high-shear emulsion machine, under 1500r/min rotating speed, disperse 55min, the sand mill sand milling 2h that is 1500r/min through rotating speed again, it is that 0.5～5 μ m, content are 20.0% fipronil bisamide and the composite suspending agent of ethyl pleocidin that screening obtains particle diameter.According to pesticide field efficacy medicine test criterion, carry out dispenser and biologically active statistics, use 4000 times of liquid of said preparation to carry out field control effectiveness test, the control efficiency of the 8th day and 12 days after the medication of cotton cotton bollworm is respectively to 87.6% and 89.5%.
Embodiment 9
Take fipronil bisamide 11.0kg, ethyl pleocidin 4.0kg, fatty alcohol-polyoxyethylene ether 5.2kg, alkyl sulfonic acid calcium 0.3kg, phenethyl phenol polyethenoxy ether sodium sulfate 0.5kg, bentonite 0.8kg, ethylene glycol 4.2kg, sodium salicylate 0.75kg, n-octyl alcohol 0.25kg and distilled water 73.0kg in high-shear emulsion machine, under 1800r/min rotating speed, disperse 50min, the sand mill sand milling 1.5h that is 1500r/min through rotating speed again, it is that 0.5～5 μ m, content are 15.0% fipronil bisamide and the composite suspending agent of ethyl pleocidin that screening obtains particle diameter.According to pesticide field efficacy medicine test criterion, carry out dispenser and biologically active statistics, use 2000 times of liquid of said preparation to carry out field control effectiveness test, the control efficiency of the 7th day and 12 days after the medication of cotton cotton bollworm is respectively to 92.3% and 94.5%.
Embodiment 10
Take fipronil bisamide 1.5kg, ethyl pleocidin 2.5kg, sodium lignin sulfonate 6.0kg, alkyl sulfonic acid calcium 1.5kg, xanthans 4.5kg, glycerine 8.0kg, potassium sorbate 0.4kg, n-octyl alcohol 0.1kg and deionized water 75.5kg in high-shear emulsion machine, under 2500r/min rotating speed, disperse 40min, the sand mill sand milling 2.5h that is 1500r/min through rotating speed again, it is that 0.5～5 μ m, content are 4.0% fipronil bisamide and the composite suspending agent of ethyl pleocidin that screening obtains particle diameter.According to pesticide field efficacy medicine test criterion, carry out dispenser and biologically active statistics, use 2000 times of liquid of said preparation to carry out field control effectiveness test, the control efficiency of the 8th day and 16 days after the medication of cotton cotton bollworm is respectively to 84.2% and 82.5%.
Embodiment 11
Take fipronil bisamide 1.2kg, ethyl pleocidin 0.8kg, Negel 3.0kg, alkylsurfuric acid calcium 2.0kg, bentonite 0.5kg, ethylene glycol 7.0kg, sodium salicylate 0.1kg, n-octyl alcohol 0.4kg and distilled water 85.0kg in high-shear emulsion machine, under 2500r/min rotating speed, disperse 40min, the sand mill sand milling 1h that is 1500r/min through rotating speed again, it is that 0.5～5 μ m, content are 2.0% fipronil bisamide and the composite suspending agent of ethyl pleocidin that screening obtains particle diameter.According to pesticide field efficacy medicine test criterion, carry out dispenser and biologically active statistics, use 1000 times of liquid of said preparation to carry out field control effectiveness test, the control efficiency of the 6th day and 12 days after the medication of wild cabbage prodenia litura is respectively to 90.3% and 88.7%.
Above embodiment shows that fipronil bisamide and the composite suspending agent disinfestation of ethyl pleocidin prepared by the present invention are effective.The composite suspending agent of the present invention is wide to control of insect spectrum, and insect is difficult to develop immunity to drugs; Preparation technology is simpler, and production cost is lower; Do not need a large amount of organic solvents, both reduced costs, reduced again organic solvent to operator's stimulation and the pollution to environment.
Claims (6)
1. the composite suspending agent of fipronil bisamide and ethyl pleocidin, it is characterized in that, by weight percentage, the raw material proportioning of described composite each component of suspending agent is: fipronil bisamide 0.2～38%, ethyl pleocidin 0.5～12%, dispersant 0.5～6%, wetting agent 0.5～5%, thickener 0.1～4.5%, antifreezing agent 2～8%, preservative 0.1～0.8%, defoamer 0.1～0.6%, water 36.0～88.0%;
Described dispersant is one or both in sodium lignin sulfonate, Negel and fatty alcohol-polyoxyethylene ether;
Described wetting agent is one or both in alkylsurfuric acid calcium, alkyl sulfonic acid calcium or phenethyl phenol polyethenoxy ether sodium sulfate;
Described thickener is bentonite or xanthans;
Described antifreezing agent is ethylene glycol or glycerine;
Described preservative is sodium salicylate or potassium sorbate;
Described defoamer is n-octyl alcohol.
2. the composite suspending agent of fipronil bisamide according to claim 1 and ethyl pleocidin, is characterized in that, described water is distilled water or deionized water.
3. the composite suspending agent of fipronil bisamide according to claim 1 and ethyl pleocidin, is characterized in that, the percentage by weight of described fipronil bisamide in raw material is 5～25%, and the percentage by weight of ethyl pleocidin in raw material is 5～10%.
4. the fipronil bisamide described in claim 1,2 or 3 and the preparation method of the composite suspending agent of ethyl pleocidin, it is characterized in that, after fipronil bisamide, ethyl pleocidin, dispersant, wetting agent, thickener, antifreezing agent, preservative, defoamer and water being mixed by raw material proportioning, shear and be dispersed to evenly, through sand milling, it is fipronil bisamide and the composite suspending agent of ethyl pleocidin of 0.5～5 μ m that screening obtains particle diameter again.
5. preparation method according to claim 4, is characterized in that, the rotating speed of described dispersion is 1000～3000r/min, and the time is 25～60min.
6. preparation method according to claim 4, is characterized in that, the rotating speed of described sand milling is 1400～1600r/min, and the time is 0.5～2.5h; It is to carry out in high-shearing dispersion emulsifying machine that described shearing disperses.
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| CN105325418A (en) * | 2015-12-16 | 2016-02-17 | 济南昊泽环保科技有限公司 | Insecticidal combination containing o-phenylenediamine insecticide and spinosad |
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| CN101669493A (en) * | 2009-10-16 | 2010-03-17 | 深圳诺普信农化股份有限公司 | Synergistic pesticide combination |
| CN101803598B (en) * | 2010-04-30 | 2013-05-29 | 江苏龙灯化学有限公司 | Low-concentration fipronil bisamide suspension agent |
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