CN102524313A - Flubendiamide and natural pyrethrins compounded suspending agent and preparation method thereof - Google Patents
Flubendiamide and natural pyrethrins compounded suspending agent and preparation method thereof Download PDFInfo
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- CN102524313A CN102524313A CN201210020908XA CN201210020908A CN102524313A CN 102524313 A CN102524313 A CN 102524313A CN 201210020908X A CN201210020908X A CN 201210020908XA CN 201210020908 A CN201210020908 A CN 201210020908A CN 102524313 A CN102524313 A CN 102524313A
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- suspending agent
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- fipronil bisamide
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
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Abstract
The invention discloses a flubendiamide and natural pyrethrins compounded suspending agent and a preparation method thereof. The compounded suspending agent is composed of flubendiamide, natural pyrethrins, dispersing agents, wetting agents, thickening agents, antifreezing agents, preservatives, antifoaming agents and water. The preparation method of the compounded suspending agent comprises adding flubendiamide, natural pyrethrins, the dispersing agents, the wetting agents, the thickening agents, the antifreezing agents, the preservatives, the antifoaming agents and the water into a high-shearing dispersing mulser, and after dispersing evenly, performing sanding and screening to obtain the flubendiamide and natural pyrethrins compounded suspending agent with the grain size to be 0.5-5mu m.The compounded suspending agent is wide in pest control spectrum, prevents pests from easily generating chemical resistance, is simple in manufacturing process and low in production cost, does not need plenty of organic solvents, reduces costs, and reduces irritation of the organic solvents on operators and pollution to the environment.
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 natural pyrethrum 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.
Natural pyrethrum is the active insecticidal components of separating and extracting from the feverfew pyrethrum flowers, comprises pyrethrin I, pyrethrin II, the plain I of cineraria, the plain II of cineraria, the plain I of jasmine chrysanthemum and the plain II of jasmine chrysanthemum.Natural pyrethrum has the effect of paralysis insect nervous centralis, belongs to the killing insects by touching agent, and is fast because of its desinsection speed, be easy to accepted by peasant household.Natural pyrethrum is one of current internationally recognized safest environmental-pollution insecticide product, is mixed with the control of insect that agricultural chemicals can be widely used in economic crops such as green vegetables, fruit, green tealeaves with it.
At present, do not see have that fipronil bisamide and natural pyrethrum 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 natural pyrethrum 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 natural pyrethrum, 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 of medicament, can delay pest resistance to insecticide.
The water-insoluble solid pesticide processing is become suspending agent, itself is 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 natural pyrethrum, by weight percentage, the each component proportioning consists of in its raw material: fipronil bisamide 0.2～30%; Natural pyrethrum 0.5～20%, dispersant 1～6%, wetting agent 1～5%; Thickener 0.1～5%, antifreezing agent 2～10%, preservative 0.1～0.7%; Antifoaming agent 0.1～1%, water 37.0～87.3%;
Said dispersant is one or both in sodium lignin sulfonate, alkyl naphthalene sulfonic acid calcium and the APES.
Said wetting agent is one or both in alkyl benzene calcium sulfonate, sodium alkyl sulfonate or the sorbitol polyoxyethylene ether;
Said thickener is xanthans or bentonite;
Said antifreezing agent is ethylene glycol or propane diols;
Said preservative is formaldehyde or Sodium Benzoate;
Said antifoaming agent is a n-octyl alcohol.
Further, said water is distilled water or deionized water.
Said fipronil bisamide accounts for 5～25% of raw material gross weight, and natural pyrethrum accounts for 5～15% of raw material gross weight.
The preparation method of described fipronil bisamide and the composite suspending agent of natural pyrethrum; May further comprise the steps: by proportioning raw materials; Fipronil bisamide, natural pyrethrum, dispersant, wetting agent, thickener, antifreezing agent, preservative, antifoaming agent and water are added in the high-shearing dispersion emulsifying machine; After being dispersed to evenly, obtaining particle diameter through sand milling, screening again is fipronil bisamide and the composite suspending agent of natural pyrethrum of 0.5～5 μ m.
Further, the rotating speed that said high-shearing dispersion emulsifying machine disperses is preferably 1000～2800r/min, and the time is 20～60min.
The rotating speed of said sand milling is preferably 1400～1600r/min, and the time is 1.5～3.0h.
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, natural pyrethrum 20.0kg, sodium lignin sulfonate 1.0kg, alkyl benzene calcium sulfonate 5.0kg, xanthans 2.5kg, ethylene glycol 4.5kg, formaldehyde 0.2kg, n-octyl alcohol 0.8kg and distilled water 65.8kg in high-shearing dispersion emulsifying machine; Under the 2800r/min rotating speed, disperse 20min; Be the sand mill sand milling 2h of 1500r/min again through rotating speed, it is that 0.5～5 μ m, content are 20.2% fipronil bisamide and the composite suspending agent of natural pyrethrum 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 6th day and 12 days after the medication of cotton cotton bollworm is respectively 91.8% and 93.5%.
Embodiment 2
Take by weighing fipronil bisamide 30.0kg, natural pyrethrum 0.5kg, alkyl naphthalene sulfonic acid calcium 3.0kg, sodium alkyl sulfonate 1.5kg, bentonite 1.2kg, propane diols 2.0kg, Sodium Benzoate 0.3kg, n-octyl alcohol 0.7kg and deionized water 60.8kg in high-shearing dispersion emulsifying machine; Under the 2600r/min rotating speed, disperse 25min; 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 30.5% fipronil bisamide and the composite suspending agent of natural pyrethrum that screening obtains particle diameter.Carry out dispenser and biologically active statistics according to the pesticide field efficacy medicine test criterion, use 3000 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 soybean prodenia litura is respectively 94.2% and 96.5%.
Embodiment 3
Take by weighing fipronil bisamide 0.2kg, natural pyrethrum 0.5kg, APES 1.5kg, sorbitol polyoxyethylene ether 2.5kg, xanthans 1.8kg, ethylene glycol 5.2kg, formaldehyde 0.4kg, n-octyl alcohol 0.6kg and distilled water 87.3kg in high-shearing dispersion emulsifying machine; Under the 2000r/min rotating speed, disperse 45min; Be the sand mill sand milling 2h 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 natural pyrethrum 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 7th day and 14 days after the medication of beet prodenia litura is respectively 82.3% and 80.5%.
Embodiment 4
Take by weighing fipronil bisamide 30.0kg, natural pyrethrum 20.0kg, sodium lignin sulfonate 3.0kg, alkyl naphthalene sulfonic acid calcium 3.0k, alkyl benzene calcium sulfonate 2.0kg, bentonite 1.0kg, propane diols 3.6kg, Sodium Benzoate 0.1kg, n-octyl alcohol 0.3kg and deionized water 37.0kg in high-shearing dispersion emulsifying machine; Under the 1000r/min rotating speed, disperse 60min; 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 50.0% fipronil bisamide and the composite suspending agent of natural pyrethrum 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; Control efficiency to the 6th day and 12 days after the medication of soybean prodenia litura is respectively 93.5% and 91.7%, and the control efficiency of the 5th day and 10 days after the medication of cotton cotton bollworm is respectively 92.9% and 94.8%.
Embodiment 5
Take by weighing fipronil bisamide 26.0kg, natural pyrethrum 18.0kg, sodium lignin sulfonate 1.0kg, APES 1.0kg, sodium alkyl sulfonate 3.0kg, xanthans 0.1kg, ethylene glycol 5.9kg, formaldehyde 0.5kg, n-octyl alcohol 0.5kg and distilled water 44.0kg in high-shearing dispersion emulsifying machine; Under the 2500r/min rotating speed, disperse 30min; Be the sand mill sand milling 3h of 1400r/min again through rotating speed, it is that 0.5～5 μ m, content are 44.0% fipronil bisamide and the composite suspending agent of natural pyrethrum 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 6th day and 12 days after the medication of beet prodenia litura is respectively 94.2% and 95.9%.
Embodiment 6
Take by weighing fipronil bisamide 22.0kg, natural pyrethrum 14.0kg, alkyl naphthalene sulfonic acid calcium 0.6kg, APES 1.0kg, sorbitol polyoxyethylene ether 2.4kg, bentonite 3.0kg, propane diols 10.0kg, Sodium Benzoate 0.6kg, n-octyl alcohol 0.4kg and deionized water 46.0kg 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 36.0% fipronil bisamide and the composite suspending agent of natural pyrethrum 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 5th day and 10 days after the medication of cotton cotton bollworm is respectively 89.4% and 92.1%.
Embodiment 7
Take by weighing fipronil bisamide 18.0kg, natural pyrethrum 12.0kg, sodium lignin sulfonate 2.2kg, alkyl benzene calcium sulfonate 1.0kg, sodium alkyl sulfonate 0.8kg, xanthans 3.2kg, ethylene glycol 3.8kg, formaldehyde 0.7kg, n-octyl alcohol 0.3kg and distilled water 58.0kg in high-shearing dispersion emulsifying machine; Under the 1500r/min rotating speed, disperse 50min; 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 30.0% fipronil bisamide and the composite suspending agent of natural pyrethrum that screening obtains particle diameter.Carry out dispenser and biologically active statistics according to the pesticide field efficacy medicine test criterion; Use 3000 times of liquid of said preparation to carry out field control effectiveness test; Control efficiency to the 7th day and 12 days after the medication of beet prodenia litura is respectively 93.5% and 94.9%, and the control efficiency of the 6th day and 10 days after the medication of cotton cotton bollworm is respectively 92.5% and 94.7%.
Embodiment 8
Take by weighing fipronil bisamide 14.0kg, natural pyrethrum 6.0kg, Negel 3.4kg, alkyl benzene calcium sulfonate 1.0kg, sorbitol polyoxyethylene ether 0.6kg, bentonite 1.5kg, propane diols 6.5kg, Sodium Benzoate 0.15kg, n-octyl alcohol 0.35kg and deionized water 66.5kg in high-shearing dispersion emulsifying machine; Under the 2000r/min rotating speed, disperse 35min; Be the sand mill sand milling 2h of 1600r/min again through rotating speed, it is that 0.5～5 μ m, content are 20.0% fipronil bisamide and the composite suspending agent of natural pyrethrum 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, the control efficiency of the 7th day and 14 days after the medication of soybean prodenia litura is respectively 83.5% and 80.1%.
Embodiment 9
Take by weighing fipronil bisamide 6.5kg, natural pyrethrum 3.5kg, APES 2.2kg, sodium alkyl sulfonate 1.8kg, sorbitol polyoxyethylene ether 1.0kg, xanthans 5.0kg, ethylene glycol 2.5kg, formaldehyde 0.25kg, n-octyl alcohol 0.75kg and distilled water 76.5kg 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 10.0% fipronil bisamide and the composite suspending agent of natural pyrethrum 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; Control efficiency to the 6th day and 12 days after the medication of cotton cotton bollworm is respectively 93.1% and 91.6%, and the control efficiency of the 5th day and 10 days after the medication of soybean prodenia litura is respectively 90.7% and 92.2%.
Embodiment 10
Take by weighing fipronil bisamide 0.5kg, natural pyrethrum 1.5kg, alkyl naphthalene sulfonic acid calcium 4.6kg, alkyl benzene calcium sulfonate 1.0kg, bentonite 2.0kg, propane diols 8.0kg, Sodium Benzoate 0.1kg, n-octyl alcohol 1.0kg and deionized water 81.3kg in high-shearing dispersion emulsifying machine; Under the 2200r/min rotating speed, disperse 30min; Be the sand mill sand milling 3h of 1500r/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 natural pyrethrum 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 beet prodenia litura is respectively 82.9% and 84.2%.
Above embodiment shows that fipronil bisamide and the composite suspending agent disinfestation of natural pyrethrum 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 natural pyrethrum is characterized in that, by weight percentage; The each component proportioning consists of in its raw material: fipronil bisamide 0.2～30%, natural pyrethrum 0.5～20%, dispersant 1～6%; Wetting agent 1～5%, thickener 0.1～5%, antifreezing agent 2～10%; Preservative 0.1～0.7%, antifoaming agent 0.1～1%, water 37.0～87.3%;
Said dispersant is one or both in sodium lignin sulfonate, alkyl naphthalene sulfonic acid calcium and the APES.
Said wetting agent is one or both in alkyl benzene calcium sulfonate, sodium alkyl sulfonate or the sorbitol polyoxyethylene ether;
Said thickener is xanthans or bentonite;
Said antifreezing agent is ethylene glycol or propane diols;
Said preservative is formaldehyde or Sodium Benzoate;
Said antifoaming agent is a n-octyl alcohol.
2. fipronil bisamide according to claim 1 and the composite suspending agent of natural pyrethrum is characterized in that said water is distilled water or deionized water.
3. fipronil bisamide according to claim 1 and the composite suspending agent of natural pyrethrum is characterized in that said fipronil bisamide accounts for 5～25% of raw material gross weight, and natural pyrethrum accounts for 5～15% of raw material gross weight.
4. the preparation method of each described fipronil bisamide of claim 1-3 and the composite suspending agent of natural pyrethrum; It is characterized in that; May further comprise the steps: by proportioning raw materials; Fipronil bisamide, natural pyrethrum, dispersant, wetting agent, thickener, antifreezing agent, preservative, antifoaming agent and water are added in the high-shearing dispersion emulsifying machine, be dispersed to evenly after, obtaining particle diameter through sand milling, screening again is fipronil bisamide and the composite suspending agent of natural pyrethrum of 0.5～5 μ m.
5. preparation method according to claim 4 is characterized in that, the rotating speed that said high-shearing dispersion emulsifying machine disperses is 1000～2800r/min, and the time is 20～60min.
6. preparation method according to claim 4 is characterized in that, the rotating speed of said sand milling is 14001600r/min, and the time is 1.5～3.0h.
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Citations (4)
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| CN101961033A (en) * | 2010-10-20 | 2011-02-02 | 华南理工大学 | Flubendiamide and natural pyrethrum compounded insect-killing microemulsion and preparation method thereof |
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2012
- 2012-01-30 CN CN201210020908XA patent/CN102524313A/en active Pending
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|---|---|---|---|---|
| CN101194611A (en) * | 2007-06-08 | 2008-06-11 | 浙江新农化工股份有限公司 | Thiazole zincium suspension agent and method for producing the same |
| US20100158965A1 (en) * | 2008-12-19 | 2010-06-24 | Else Beitzel | Window sticker for attracting and destroying insects |
| CN101755750A (en) * | 2009-11-17 | 2010-06-30 | 陕西汤普森生物科技有限公司 | Insecticide containing flubendiamide |
| CN101961033A (en) * | 2010-10-20 | 2011-02-02 | 华南理工大学 | Flubendiamide and natural pyrethrum compounded insect-killing microemulsion and preparation method thereof |
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Application publication date: 20120704 |