CN102578117A - Flubendiamide-rotenone compound suspending agent and preparation method thereof - Google Patents
Flubendiamide-rotenone compound suspending agent and preparation method thereof Download PDFInfo
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- CN102578117A CN102578117A CN2012100194258A CN201210019425A CN102578117A CN 102578117 A CN102578117 A CN 102578117A CN 2012100194258 A CN2012100194258 A CN 2012100194258A CN 201210019425 A CN201210019425 A CN 201210019425A CN 102578117 A CN102578117 A CN 102578117A
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Abstract
The invention discloses a flubendiamide-rotenone compound suspending agent and a preparation method thereof. The compound suspending agent consists of flubendiamide, rotenone, a dispersing agent, a wetting agent, a thickener, an anti-freezing agent, a preservative, a defoaming agent and water. The preparation method of the compound suspending agent comprises the following steps of: adding the flubendiamide, rotenone, dispersing agent, wetting agent, thickener, anti-freezing agent, preservative, defoaming agent and water into a high-shear dispersing emulsifying machine; dispersing uniformly; and grinding and sieving to obtain the flubendiamide-rotenone compound suspending agent of which the grain diameter is 0.5-5 mum. The compound suspending agent has a wide pest prevention and control spectrum, and the drug resistance of pests is avoided; the preparation process is simple, and is low in production cost; and a large quantity of organic solvents are not required, the cost is lowered, and the stimulation of organic solvents to operators and environmental pollution caused by the organic solvents are lowered.
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 rotenone and preparation method thereof.
Background technology
Contain a large amount of organic solvents in the chemical pesticide, when making huge contribution, also brought serious pollution to natural environment for agricultural foison.Along with environmental regulation becomes better and approaching perfection day by day, the cry that reduces pesticide pollution is strong day by day.Develop safely, environmental protection and cheap novel liquid formulation are to reduce or eliminate the trend of the times of organic solvent harm having become agricultural chemicals development.Wherein, Water-borne modification is exactly one of dominant direction of formulations of pesticide development.This type pesticides new formulation also can increase new characteristic to agricultural chemicals; More can give full play to the function Characteristics of former medicine self, overcome and remedy the deficiency of the original formulation of agricultural chemicals, all lower to people and animals' toxicity and excitant; And can alleviate poisoning to crop; Improve physico chemistry and biological property, expanding application scope, the service life of prolongation medicament.
Agricultural chemicals suspension agent belongs to one of Water-borne modification novel form, is pesticide active ingredient and dispersant, wetting agent, thickener, antifoaming agent, antifreezing agent etc. are dispersed in the matrix water and the high dispersive that forms, stable suspended substance.Agricultural chemicals suspension agent has the advantage of wetting powder and missible oil concurrently: aspect drug effect, the suspending agent herbicide effects is superior to wetting powder, and the insecticide effect is then close with missible oil; Because agricultural chemicals suspension agent is dispersion medium with water, make it have environmental protection, cheap characteristics, reduced the use of a large amount of organic solvents simultaneously, production process safety, pollution-free; And suspending agent can mix with arbitrary proportion with water, and is easy to use, can reach bigger coverage rate after the dilution, can be processed to the formulation of high concentration.
The fipronil bisamide chemical name is 3-iodo-N '-(2-mesyl)-1,1-dimethyl ethyl group-N-{4-[1,2,2,2-tetrafluoro-1-(trifluoromethyl) ethyl]-0-tolyl } phthalic amide.Belong to novel phthalic amide insecticides, insect ryania (muscle) receptor activators, different fully with the mechanism of action of insecticide in the past, can make excessively to discharge calcium ion in the insect bodies, cause insect death.This insecticide does not produce cross resistance with existing insecticide, and efficient, safety, is rising novel pesticide.
Rotenone belongs to flavonoids, and chemical name is [2R-(2 α, 6a α, 12a α)]-1; 2.12,12a-tetrahydrochysene-8,9-dimethoxy-2-(1-methoxy vinyl)-[I]-chromene [3; 4-b]-furans also-[2,3-h] [1]-chromenes-6 (6aH)-ketone, mainly come from the plants such as trifoliate jewelvine, Africa mountain soya bean; Its insecticidal action mechanism is special, and insect is had significant stomach toxicity and contact toxicity, and has food refusal and the inhibition activity of growing concurrently.Can be used for the various pests control on vegetables, fruit tree, paddy rice, tea tree, tobacco and the cotton.
At present, do not see have that fipronil bisamide and rotenone are composite to be the report of suspending agent.
Summary of the invention
The objective of the invention is the deficiency to prior art, provide a kind of wide to the control of insect spectrum, insect is difficult to develop immunity to drugs, and the fipronil bisamide of safety and environmental protection and the composite suspending agent of rotenone 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 rotenone, and the two is composite for not only having enlarged the control of insect spectrum behind the suspending agent, and has increased the action target spot to medicament, can delay pest resistance to insecticide.
With the suspending agent that the water-insoluble solid pesticide processing becomes, itself be a kind of thermodynamic unstable system between colloid and rough segmentation system.The present invention is added with auxiliary agents such as wetting agent, dispersant and antifreezing agent in the preparation process of suspending agent, the main effect of wetting agent and dispersant is: increase the dispersion medium viscosity, reduce the difference in specific gravity between dispersion medium and the disperse phase.Coordinate each other through auxiliary agent and active component, kept stability of formulation.The prepared suspending agent of the present invention has that particle diameter is little, biologically active is high and characteristics such as using dosage is low, and is medium with water, and it is environmentally friendly.
For reaching above purpose, the present invention has adopted following technical scheme:
The composite suspending agent of fipronil bisamide and rotenone, by weight percentage, the each component proportioning consists of in its raw material: fipronil bisamide 0.2～35%; Rotenone 0.5～15%, dispersant 0.5～5%, wetting agent 1～4%; Thickener 0.1～3.5%, antifreezing agent 1～10%, preservative 0.1～1%; Antifoaming agent 0.1～0.8%, water 38.4～88.6%;
Said dispersant is one or both in calcium lignosulfonate, alkyl naphthalene sulfonic acid calcium or the APES;
Said wetting agent is one or both in sodium alkyl benzene sulfonate, alkyl sulfonic acid calcium or the sorbitol polyoxyethylene base ether;
Said thickener is polyvinyl alcohol or carboxymethyl cellulose;
Said antifreezing agent is urea or propane diols;
Said preservative is formaldehyde or sodium salicylate;
Said antifoaming agent is polyethers-silicone antifoam agent.
Further, said water is preferably distilled water or deionized water.
Said fipronil bisamide preferably accounts for 5～30% of material component gross weight, and rotenone preferably accounts for 5～10% of material component gross weight.
The preparation method of described fipronil bisamide and the composite suspending agent of rotenone; Press the material component proportioning with fipronil bisamide, rotenone, dispersant, wetting agent, thickener, antifreezing agent, preservative, antifoaming agent and water mixed and dispersed after evenly, obtaining particle diameter through sand milling, screening again is fipronil bisamide and the composite suspending agent of rotenone of 0.5～5 μ m.
Further, said dispersion is preferably carried out at high-shearing dispersion emulsifying machine, and rotating speed is preferably 1200～2800r/min, and the time is 35～60min.
The rotating speed of said sand milling is preferably 1400～1600r/min, and the time is 1.0～2.5h.
The present invention compared with prior art has following advantage:
(1) the composite suspending agent of the present invention is wide to the 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) do not use a large amount of organic solvents in the production process of the composite suspending agent of the present invention, safety and environmental protection, environmental pollution is little;
(4) the composite suspending agent of the present invention does not contain 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 present invention is described further, but the scope that the present invention requires to protect is not limited thereto.
Embodiment 1
Take by weighing fipronil bisamide 0.2kg, rotenone 15.0kg, calcium lignosulfonate 3.0kg, sodium alkyl benzene sulfonate 1.0kg, polyvinyl alcohol 1.4kg, urea 4.6kg, formaldehyde 0.8kg, polyethers-silicone antifoam agent 0.2kg and distilled water 73.8kg in high-shearing dispersion emulsifying machine; Under the 2000r/min rotating speed, disperse 40min; Be the sand mill sand milling 2h of 1500r/min again through rotating speed, it is that 0.5～5 μ m, content are 15.2% fipronil bisamide and the composite suspending agent of rotenone that screening obtains particle diameter.Carry out dispenser and biologically active statistics according to the pesticide field efficacy medicine test criterion, 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 beet armyworm is respectively 92.2% and 94.7%.
Embodiment 2
Take by weighing fipronil bisamide 35.0kg, rotenone 0.5kg, alkyl naphthalene sulfonic acid calcium 3.5kg, alkyl sulfonic acid calcium 1.5kg, carboxymethyl cellulose 1.2kg, propane diols 3.8kg, sodium salicylate 0.7kg, polyethers-silicone antifoam agent 0.3kg and deionized water 53.5kg in high-shearing dispersion emulsifying machine; Under the 2800r/min rotating speed, disperse 35min; Be the sand mill sand milling 2.5h of 1400r/min again through rotating speed, it is that 0.5～5 μ m, content are 35.5% fipronil bisamide and the composite suspending agent of rotenone that screening obtains particle diameter.Carry out dispenser and biologically active statistics according to the pesticide field efficacy medicine test criterion, use 4000 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 beet armyworm is respectively 91.9% and 93.5%.
Embodiment 3
Take by weighing fipronil bisamide 0.2kg, rotenone 0.5kg, APES 1.2kg, sorbitol polyoxyethylene ether 1.8kg, polyvinyl alcohol 2.0kg, urea 5.2kg, formaldehyde 0.1kg, polyethers-silicone antifoam agent 0.4kg and distilled water 88.6kg in high-shearing dispersion emulsifying machine; Under the 2000r/min rotating speed, disperse 45min; Be the sand mill sand milling 1.5h of 1500r/min again through rotating speed, it is that 0.5～5 μ m, content are 0.7% fipronil bisamide and the composite suspending agent of rotenone that screening obtains particle diameter.Carry out dispenser and biologically active statistics according to the pesticide field efficacy medicine test criterion, use 1200 times of liquid of said preparation to carry out field control effectiveness test, the control efficiency of the 7th day and 14 days after the medication of Chinese cabbage beet armyworm is respectively 85.5% and 82.8%.
Embodiment 4
Take by weighing fipronil bisamide 35.0kg, rotenone 15.0kg, calcium lignosulfonate 2.5kg, alkyl naphthalene sulfonic acid calcium 2.0k, sodium alkyl benzene sulfonate 3.5kg, carboxymethyl cellulose 1.6kg, propane diols 1.0kg, sodium salicylate 0.5kg, polyethers-silicone antifoam agent 0.5kg and deionized water 38.4kg in high-shearing dispersion emulsifying machine; Under the 1800r/min rotating speed, disperse 60min; Be the sand mill sand milling 2h of 1500r/min again through rotating speed, it is that 0.5～5 μ m, content are 50.0% fipronil bisamide and the composite suspending agent of rotenone that screening obtains particle diameter.Carry out dispenser and biologically active statistics according to the pesticide field efficacy medicine test criterion, use 5000 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 cabbage aphid medication is respectively 93.7% and 92.5%.
Embodiment 5
Take by weighing fipronil bisamide 30.0kg, rotenone 12.0kg, calcium lignosulfonate 1.5kg, APES 3.5kg, alkyl sulfonic acid calcium 2.0kg, polyvinyl alcohol 1.5kg, urea 2.5kg, formaldehyde 0.2kg, polyethers-silicone antifoam agent 0.8kg and distilled water 46.0kg in high-shearing dispersion emulsifying machine; Under the 2200r/min rotating speed, disperse 40min; Be the sand mill sand milling 1.5h of 1600r/min again through rotating speed, it is that 0.5～5 μ m, content are 42.0% fipronil bisamide and the composite suspending agent of rotenone that screening obtains particle diameter.Carry out dispenser and biologically active statistics according to the pesticide field efficacy medicine test criterion; Use 4500 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 Chinese cabbage beet armyworm is respectively 93.2% and 95.5%, and the control efficiency of the 7th day and 12 days after the cabbage aphid medication is respectively 93.0% and 95.2%.
Embodiment 6
Take by weighing fipronil bisamide 28.0kg, rotenone 10.0kg, Negel 0.4kg, APES 0.1kg, sorbitol polyoxyethylene ether 2.5kg, carboxymethyl cellulose 0.1kg, propane diols 3.5kg, sodium salicylate 0.6kg, polyethers-silicone antifoam agent 0.4kg and deionized water 54.4kg in high-shearing dispersion emulsifying machine; Under the 2500r/min rotating speed, disperse 40min; Be the sand mill sand milling 2.5h of 1500r/min again through rotating speed, it is that 0.5～5 μ m, content are 38.0% fipronil bisamide and the composite suspending agent of rotenone that screening obtains particle diameter.Carry out dispenser and biologically active statistics according to the pesticide field efficacy medicine test criterion, 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 wild cabbage beet armyworm is respectively 92.6% and 94.3%.
Embodiment 7
Take by weighing fipronil bisamide 23.0kg, rotenone 8.0kg, calcium lignosulfonate 1.0kg, sodium alkyl benzene sulfonate 2.0kg, alkyl sulfonic acid calcium 2.0kg, polyvinyl alcohol 0.3kg, urea 8.0kg, formaldehyde 0.4kg, polyethers-silicone antifoam agent 0.3kg and distilled water 55.0kg in high-shearing dispersion emulsifying machine; Under the 1800r/min rotating speed, disperse 50min; Be the sand mill sand milling 1h of 1600r/min again through rotating speed, it is that 0.5～5 μ m, content are 31.0% fipronil bisamide and the composite suspending agent of rotenone that screening obtains particle diameter.Carry out dispenser and biologically active statistics according to the pesticide field efficacy medicine test criterion; Use 3500 times of liquid of said preparation to carry out field control effectiveness test; Control efficiency to the 6th day and 12 days after the medication of wild cabbage beet armyworm is respectively 95.3% and 97.4%, and the control efficiency of the 7th day and 14 days after the cabbage aphid medication is respectively 92.7% and 90.8%.
Embodiment 8
Take by weighing fipronil bisamide 18.0kg, rotenone 5.0kg, Negel 2.4kg, sodium alkyl benzene sulfonate 1.0kg, sorbitol polyoxyethylene ether 0.6kg, carboxymethyl cellulose 3.0kg, propane diols 6.0kg, sodium salicylate 0.3kg, polyethers-silicone antifoam agent 0.6kg and deionized water 63.1kg in high-shearing dispersion emulsifying machine; Under the 1500r/min rotating speed, disperse 55min; Be the sand mill sand milling 2h of 1500r/min again through rotating speed, it is that 0.5～5 μ m, content are 23.0% fipronil bisamide and the composite suspending agent of rotenone that screening obtains particle diameter.Carry out dispenser and biologically active statistics according to the pesticide field efficacy medicine test criterion, use 4000 times of liquid of said preparation to carry out field control effectiveness test, the control efficiency of the 7th day and 10 days after the medication of Chinese cabbage beet armyworm is respectively 88.7% and 90.6%.
Embodiment 9
Take by weighing fipronil bisamide 12.0kg, rotenone 3.0kg, APES 3.6kg, alkyl sulfonic acid calcium 0.5kg, sorbitol polyoxyethylene ether 0.9kg, polyvinyl alcohol 2.4kg, urea 1.6kg, formaldehyde 1.0kg, polyethers-silicone antifoam agent 0.1kg and distilled water 74.9kg in high-shearing dispersion emulsifying machine; Under the 2000r/min rotating speed, disperse 55min; Be the sand mill sand milling 1.5h of 1500r/min again through rotating speed, it is that 0.5～5 μ m, content are 15.0% fipronil bisamide and the composite suspending agent of rotenone that screening obtains particle diameter.Carry out dispenser and biologically active statistics according to the pesticide field efficacy medicine test criterion; Use 2000 times of liquid of said preparation to carry out field control effectiveness test; Control efficiency to the 8th day and 16 days after the cabbage aphid medication is respectively 91.8% and 80.2%, and the control efficiency of the 6th day and 12 days after the medication of Chinese cabbage beet armyworm is respectively 94.0% and 95.4%.
Embodiment 10
Take by weighing fipronil bisamide 0.8kg, rotenone 1.2kg, alkyl naphthalene sulfonic acid calcium 0.8kg, sodium alkyl benzene sulfonate 2.2kg, carboxymethyl cellulose 3.5kg, propane diols 10.0kg, sodium salicylate 0.15kg, polyethers-silicone antifoam agent 0.25kg and deionized water 81.1kg in high-shearing dispersion emulsifying machine; Under the 1200r/min rotating speed, disperse 60min; Be the sand mill sand milling 2.0h of 1400r/min again through rotating speed, it is that 0.5～5 μ m, content are 2.0% fipronil bisamide and the composite suspending agent of rotenone that screening obtains particle diameter.Carry out dispenser and biologically active statistics according to the pesticide field efficacy medicine test criterion, use 1500 times of liquid of said preparation to carry out field control effectiveness test, the control efficiency of the 7th day and 10 days after the cabbage aphid medication is respectively 91.5% and 90.2%.
Above embodiment shows that fipronil bisamide and the composite suspending agent disinfestation of rotenone that the present invention prepares are effective.The composite suspending agent of the present invention is wide to the 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 cost, reduced organic solvent again to operator's stimulation with to the pollution of environment.
Claims (6)
1. the composite suspending agent of fipronil bisamide and rotenone is characterized in that, by weight percentage; The each component proportioning consists of in its raw material: fipronil bisamide 0.2～35%, rotenone 0.5～15%, dispersant 0.5～5%; Wetting agent 1～4%, thickener 0.1～3.5%, antifreezing agent 1～10%; Preservative 0.1～1%, antifoaming agent 0.1～0.8%, water 38.4～88.6%;
Said dispersant is one or both in calcium lignosulfonate, alkyl naphthalene sulfonic acid calcium or the APES;
Said wetting agent is one or both in sodium alkyl benzene sulfonate, alkyl sulfonic acid calcium or the sorbitol polyoxyethylene base ether;
Said thickener is polyvinyl alcohol or carboxymethyl cellulose;
Said antifreezing agent is urea or propane diols;
Said preservative is formaldehyde or sodium salicylate;
Said antifoaming agent is polyethers-silicone antifoam agent.
2. described fipronil bisamide of claim 1 and the composite suspending agent of rotenone is characterized in that, said water is distilled water or deionized water.
3. described fipronil bisamide of claim 1 and the composite suspending agent of rotenone is characterized in that said fipronil bisamide accounts for 5～30% of material component gross weight, and rotenone accounts for 5～10% of material component gross weight.
4. the preparation method of each described fipronil bisamide of claim 1-3 and the composite suspending agent of rotenone; It is characterized in that; Press the material component proportioning with fipronil bisamide, rotenone, dispersant, wetting agent, thickener, antifreezing agent, preservative, antifoaming agent and water mixed and dispersed after evenly, obtaining particle diameter through sand milling, screening again is fipronil bisamide and the composite suspending agent of rotenone of 0.5～5 μ m.
5. preparation method according to claim 4 is characterized in that, said dispersion is to carry out at high-shearing dispersion emulsifying machine, and rotating speed is 1200～2800r/min, and the time is 35～60min.
6. preparation method according to claim 4 is characterized in that, the rotating speed of said sand milling is 1400～1600r/min, and the time is 1.0～2.5h.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2012100194258A CN102578117A (en) | 2012-01-19 | 2012-01-19 | Flubendiamide-rotenone compound suspending agent and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN2012100194258A CN102578117A (en) | 2012-01-19 | 2012-01-19 | Flubendiamide-rotenone compound suspending agent and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104521967A (en) * | 2014-12-08 | 2015-04-22 | 海南正业中农高科股份有限公司 | Agricultural composition containing flubendiamide and plant-derived substances, and applications thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6603044B1 (en) * | 1998-11-30 | 2003-08-05 | Nihon Nohyaku Co., Ltd. | Phthalamide derivatives, or salt thereof agrohorticultural insecticide, and method for using the same |
| CN101836643A (en) * | 2010-06-01 | 2010-09-22 | 扬州大学 | Pesticide preparation for controlling vegetable pests of diamondback moth and the like |
| CN101971833A (en) * | 2010-10-20 | 2011-02-16 | 华南理工大学 | Flubendiamide and rotenone compound insecticidal water dispersible granule and preparation method thereof |
-
2012
- 2012-01-19 CN CN2012100194258A patent/CN102578117A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6603044B1 (en) * | 1998-11-30 | 2003-08-05 | Nihon Nohyaku Co., Ltd. | Phthalamide derivatives, or salt thereof agrohorticultural insecticide, and method for using the same |
| CN101836643A (en) * | 2010-06-01 | 2010-09-22 | 扬州大学 | Pesticide preparation for controlling vegetable pests of diamondback moth and the like |
| CN101971833A (en) * | 2010-10-20 | 2011-02-16 | 华南理工大学 | Flubendiamide and rotenone compound insecticidal water dispersible granule and preparation method thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104521967A (en) * | 2014-12-08 | 2015-04-22 | 海南正业中农高科股份有限公司 | Agricultural composition containing flubendiamide and plant-derived substances, and applications thereof |
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