Summary of the invention
The object of the invention is to overcome the shortcoming that prior art exists, a kind of high-efficiency low-toxicity, low cost, environmentally friendly are provided, can prevent and treat beet armyworm, diamond-back moth, cotton bollworm and the significant fipronil bisamide of cabbage aphid effect and rotenone and composite water dispersible granules novel agrochemical insecticide.
Another object of the present invention is to provide the preparation method of above-mentioned fipronil bisamide and the composite water dispersible granule insecticide of rotenone.
The composite use of fipronil bisamide and rotenone, can work in coordination with and play a role, and improves insecticide efficiency, strengthens control efficiency, delays pest resistance to insecticide, has made up self deficiency of single dose agricultural chemicals.
The composite water dispersible granules of fipronil bisamide and rotenone, in formula, the percentage by weight of each component is: fipronil bisamide 0.1%-65%, rotenone 5%-15%, dispersant 3%-25%, wetting agent 3%-5%, disintegrant 1%-25%, binding agent 0.1%-0.5%, stabilizing agent 0.1%-0.5%, carrier 10%-60%.
Described dispersant is one or more in acrylate homopolymer sodium salt, phenethyl phenol polyethenoxy sodium sulphate, sodium lignin sulfonate, Fluhyzon formaldehyde condensation products, alkylbenzenesulfonate, alkylphenol polyoxyethylene formaldehyde condensation products.
Described wetting agent is one or more in sodium alkyl sulfate, alkylnaphthalene sulfonate, benzyl naphthalene sulfonate, benzyl naphthalenesulfonate formaldehyde condensation compound, dialkyl group naphthalene sulfonate, fatty acid amide N methyl taurine salt.
Described disintegrant is one or more in ammonium sulfate, bentonite, polyethylene glycol, modified starch, White Carbon black, silica gel.
Described binding agent is one or more in Sodium Polyacrylate, wooden sodium, dextrin, sodium carboxymethylcellulose, xanthans.
Described stabilizing agent is one or more in niter cake, another name for sodium, citric acid, carbonic hydroammonium, sodium hydroxide.
Described carrier is one or more in kaolin, diatomite, clay, Emathlite, mica powder, sepiolite, calcium carbonate.
The preparation technology of described fipronil bisamide and the composite water dispersible granules of rotenone is:
1, the composite water dispersible granules formula material of one group of fipronil bisamide and rotenone is mixed;
2, formula material is ground into female powder through micro jet;
3, female powder is mixed with deionized water, then the granulation of rotating disk squash type;
4, granulation profile is defective returns to granulation, and profile is qualified, and to enter drier dry;
5, dry, screening, packing after inspection by sampling is qualified.
Water dispersible granules of the present invention is to contain active insecticidal components fipronil bisamide and rotenone.
The present invention utilizes derris root or Leaves of Tephrosia vogelii Hook f to carry out lixiviate, extracts solvent and can select a kind of in methyl alcohol, ethanol and chloroform, and extract becomes the concentrated extract that contains rotenone after reduced pressure concentration.
The composite water dispersible granules of fipronil bisamide of the present invention and rotenone compared with prior art, has suspensibility high, and heat storage stability is good, disintegration rate is fast, good dispersion; The composite water dispersible granules of fipronil bisamide of the present invention and rotenone, to environment, people and animals and other beneficial organism safety, is difficult for producing poisoning; Preparation technology is comparatively simple, easy to use, with low cost, is suitable for suitability for industrialized production and large scale application.
Embodiment
For a better understanding of the present invention, below in conjunction with embodiment, the invention will be further described, but the scope of protection of present invention is not limited to the scope that embodiment represents.
Embodiment 1: take fipronil bisamide 0.1kg and rotenone 5.0kg, then with phenethyl phenol polyethenoxy sodium sulphate 12.0kg, sodium alkyl sulfate 5.0kg, ammonium sulfate 20.0kg, sodium carboxymethylcellulose 0.1kg, citric acid 0.2kg, mica powder 20.0kg and kaolin 37.6kg.After mixing, through micro jet, be ground into female powder, add again 5.0kg deionized water to mix in female powder, granulation, dry, screening, by the qualified packing of sample analysis, is made the composite water dispersible granules of fipronil bisamide and rotenone.Through check moisture < 2%, lasting foaming characteristic (1min) < 7ml, wetability < 40s, acceleration heat storage stability is qualified.Dilute with water said preparation carries out field control effectiveness test, its 1500 times of liquid to cabbage aphid medication after the control efficiency of the 5th day and 10 days be respectively 87.5% and 84.1%, control efficiency to the 7th day and 14 days after beet armyworm medication is respectively 88.1% and 85.2%, and the control efficiency of the 6th day and 12 days after cotton bollworm medication is respectively to 90.0% and 88.8%.
Embodiment 2: take fipronil bisamide 0.1kg and rotenone 15.0kg, then with acrylate homopolymer sodium salt 15.0kg, alkylnaphthalene sulfonate 5.0kg, bentonite 22.0kg, Sodium Polyacrylate 0.2kg, niter cake 0.1kg, diatomite 20.0kg and calcium carbonate 22.6kg.After mixing, through micro jet, be ground into female powder, add again 3.5kg deionized water to mix in female powder, granulation, dry, screening, by the qualified packing of sample analysis, is made the composite water dispersible granules of fipronil bisamide and rotenone.Through check moisture < 2%, lasting foaming characteristic (1min) < 7ml, wetability < 40s, acceleration heat storage stability is qualified.Dilute with water said preparation carries out field control effectiveness test, its 1500 times of liquid to cabbage aphid medication after the control efficiency of the 5th day and 10 days be respectively 90.2% and 92.3%, control efficiency to the 7th day and 14 days after beet armyworm medication is respectively 92.4% and 94.0%, and the control efficiency of the 6th day and 12 days after cotton bollworm medication is respectively to 94.0% and 90.5%.
Embodiment 3: take fipronil bisamide 65.0kg and rotenone 15.0kg, then with sodium lignin sulfonate 2.0kg, benzyl naphthalene sulfonate 2.5kg, polyethylene glycol 5.0kg, dextrin 0.2kg, another name for sodium 0.3kg and bentonite 10.0kg.After mixing, through micro jet, be ground into female powder, add again 4.0kg deionized water to mix in female powder, granulation, dry, screening, by the qualified packing of sample analysis, is made the composite water dispersible granules of fipronil bisamide and rotenone.Through check moisture < 2%, lasting foaming characteristic (1min) < 7ml, wetability < 40s, acceleration heat storage stability is qualified.Dilute with water said preparation carries out field control effectiveness test, its 3000 times of liquid to cabbage aphid medication after the control efficiency of the 5th day and 10 days be respectively 91.5% and 92.8%, control efficiency to the 7th day and 14 days after beet armyworm medication is respectively 91.8% and 93.2%, and the control efficiency of the 6th day and 12 days after cotton bollworm medication is respectively to 93.1% and 90.7%.
Embodiment 4: take fipronil bisamide 65.0kg and rotenone 5.0kg, then with Fluhyzon formaldehyde condensation products 5.0kg, benzyl naphthalenesulfonate formaldehyde condensation compound 3.5kg, silica gel 3.5kg, xanthans 0.5kg, carbonic hydroammonium 0.2kg and clay 17.3kg.After mixing, through micro jet, be ground into female powder, add again 5.5kg deionized water to mix in female powder, granulation, dry, screening, by the qualified packing of sample analysis, is made the composite water dispersible granules of fipronil bisamide and rotenone.Through check moisture < 2%, lasting foaming characteristic (1min) < 7ml, wetability < 40s, acceleration heat storage stability is qualified.Dilute with water said preparation carries out field control effectiveness test, its 2500 times of liquid to cabbage aphid medication after the control efficiency of the 5th day and 10 days be respectively 91.1% and 92.3%, control efficiency to the 7th day and 14 days after beet armyworm medication is respectively 91.3% and 93.0%, and the control efficiency of the 6th day and 12 days after cotton bollworm medication is respectively to 92.2% and 90.2%.
Embodiment 5: take fipronil bisamide 1.0kg and rotenone 5.5kg, then with alkylbenzenesulfonate 15.0kg, dialkyl group naphthalene sulfonate 3.0kg, modified starch 15.0kg, xanthans 0.1kg, sodium hydroxide 0.1kg, clay 27.3kg and sepiolite 33.0kg.After mixing, through micro jet, be ground into female powder, add again 6.0kg deionized water to mix in female powder, granulation, dry, screening, by the qualified packing of sample analysis, is made the composite water dispersible granules of fipronil bisamide and rotenone.Through check moisture < 2%, lasting foaming characteristic (1min) < 7ml, wetability < 40s, acceleration heat storage stability is qualified.Dilute with water said preparation carries out field control effectiveness test, its 1500 times of liquid to cabbage aphid medication after the control efficiency of the 5th day and 10 days be respectively 89.1% and 90.3%, control efficiency to the 7th day and 14 days after beet armyworm medication is respectively 88.3% and 89.5%, and the control efficiency of the 6th day and 12 days after cotton bollworm medication is respectively to 89.2% and 90.5%.
Embodiment 6: take fipronil bisamide 5.0kg and rotenone 5.0kg, then with alkylphenol polyoxyethylene formaldehyde condensation products 20.0kg, fatty acid amide N methyl taurine salt 4.5kg, White Carbon black 16.5kg, dextrin 0.3kg, xanthans 0.1kg, niter cake 0.5kg, Emathlite 48.1kg.After mixing, through micro jet, be ground into female powder, add again 9.5kg deionized water to mix in female powder, granulation, dry, screening, by the qualified packing of sample analysis, is made the composite water dispersible granules of fipronil bisamide and rotenone.Through check moisture < 2%, lasting foaming characteristic (1min) < 7ml, wetability < 40s, acceleration heat storage stability is qualified.Dilute with water said preparation carries out field control effectiveness test, its 1500 times of liquid to cabbage aphid medication after the control efficiency of the 5th day and 10 days be respectively 91.3% and 92.5%, control efficiency to the 7th day and 14 days after beet armyworm medication is respectively 89.6% and 90.5%, and the control efficiency of the 6th day and 12 days after cotton bollworm medication is respectively to 89.8% and 91.3%.
Embodiment 7: take fipronil bisamide 10.0kg and rotenone 5.0kg, then with acrylate homopolymer sodium salt 5kg, alkylphenol polyoxyethylene formaldehyde condensation products 13.0kg, benzyl naphthalene sulfonate 1.5kg, sodium alkyl sulfate 1.0kg, silica gel 15.0kg, dextrin 0.2kg, polyethylene glycol 0.2kg, another name for sodium 0.2kg, niter cake 0.3kg, Emathlite 20.0kg, kaolin 10.0kg and clay 18.6kg.After mixing, through micro jet, be ground into female powder, add again 10.0kg deionized water to mix in female powder, granulation, dry, screening, by the qualified packing of sample analysis, is made the composite water dispersible granules of fipronil bisamide and rotenone.Through check moisture < 2%, lasting foaming characteristic (1min) < 7ml, wetability < 40s, acceleration heat storage stability is qualified.Dilute with water said preparation carries out field control effectiveness test, its 1500 times of liquid to cabbage aphid medication after the control efficiency of the 5th day and 10 days be respectively 95.3% and 93.2%, control efficiency to the 7th day and 14 days after beet armyworm medication is respectively 94.3% and 95.3%, and the control efficiency of the 6th day and 12 days after cotton bollworm medication is respectively to 95.4% and 96.9%.
Embodiment 8: take fipronil bisamide 10.0kg and rotenone 10.0kg, then with Fluhyzon formaldehyde condensation products 5.0kg, acrylate homopolymer sodium salt 10.0kg, dialkyl group sulfonate 2.5kg, silica gel 15.0kg, dextrin 0.5kg, another name for sodium 0.2kg, kaolin 20.0kg and clay 26.8kg.After mixing, through micro jet, be ground into female powder, add again 6.5kg deionized water to mix in female powder, granulation, dry, screening, by the qualified packing of sample analysis, is made the composite water dispersible granules of fipronil bisamide and rotenone.Through check moisture < 2%, lasting foaming characteristic (1min) < 7ml, wetability < 40s, acceleration heat storage stability is qualified.Dilute with water said preparation carries out field control effectiveness test, its 1500 times of liquid to cabbage aphid medication after the control efficiency of the 5th day and 10 days be respectively 96.6% and 97.6%, control efficiency to the 7th day and 14 days after beet armyworm medication is respectively 98.2% and 98.7%, and the control efficiency of the 6th day and 12 days after cotton bollworm medication is respectively to 96.8% and 97.7%.
Embodiment 9: take fipronil bisamide 18.0kg and rotenone 15.0kg, then with sodium lignin sulfonate 10.0kg, benzyl naphthalene sulfonate 4.5kg, polyethylene glycol 20.0kg, dextrin 0.2kg, another name for sodium 0.3kg and bentonite 32.0kg.After mixing, through micro jet, be ground into female powder, add again 6.0kg deionized water to mix in female powder, granulation, dry, screening, by the qualified packing of sample analysis, is made the composite water dispersible granules of fipronil bisamide and rotenone.Through check moisture < 2%, lasting foaming characteristic (1min) < 7ml, wetability < 40s, acceleration heat storage stability is qualified.Dilute with water said preparation carries out field control effectiveness test, its 3000 times of liquid to cabbage aphid medication after the control efficiency of the 5th day and 10 days be respectively 91.0% and 92.3%, control efficiency to the 7th day and 14 days after beet armyworm medication is respectively 91.2% and 92.6%, and the control efficiency of the 6th day and 12 days after cotton bollworm medication is respectively to 92.1% and 90.4%.
Embodiment 10: take fipronil bisamide 13.5kg and rotenone 10.0kg, then with sodium lignin sulfonate 10.0kg, benzyl naphthalene sulfonate 4.5kg, polyethylene glycol 20.0kg, dextrin 0.2kg, another name for sodium 0.3kg and bentonite 41.5kg.After mixing, through micro jet, be ground into female powder, female powder added to 5.6kg again and enter deionized water and mix, granulation, dry, screening, by the qualified packing of sample analysis, is made the composite water dispersible granules of fipronil bisamide and rotenone.Through check moisture < 2%, lasting foaming characteristic (1min) < 7ml, wetability < 40s, acceleration heat storage stability is qualified.Dilute with water said preparation carries out field control effectiveness test, its 3000 times of liquid to cabbage aphid medication after the control efficiency of the 5th day and 10 days be respectively 91.0% and 92.4%, control efficiency to the 7th day and 14 days after beet armyworm medication is respectively 91.2% and 93.0%, and the control efficiency of the 6th day and 12 days after cotton bollworm medication is respectively to 92.4% and 90.1%.
Embodiment 11: take fipronil bisamide 8.5kg and rotenone 9.0kg, then with alkylphenol polyoxyethylene formaldehyde condensation products 20.0kg, fatty acid amide N methyl taurine salt 4.5kg, White Carbon black 16.5kg, dextrin 0.3kg, xanthans 0.1kg, niter cake 0.5kg, mica powder 20.6kg and Emathlite 20.0kg.After mixing, through micro jet, be ground into female powder, add again 8.5kg deionized water to mix in female powder, granulation, dry, screening, by the qualified packing of sample analysis, is made the composite water dispersible granules of fipronil bisamide and rotenone.Through check moisture < 2%, lasting foaming characteristic (1min) < 7ml, wetability < 40s, acceleration heat storage stability is qualified.Dilute with water said preparation carries out field control effectiveness test, its 1500 times of liquid to cabbage aphid medication after the control efficiency of the 5th day and 10 days be respectively 91.7% and 93.1%, control efficiency to the 7th day and 14 days after beet armyworm medication is respectively 90.6% and 91.5%, and the control efficiency of the 6th day and 12 days after cotton bollworm medication is respectively to 90.8% and 91.9%.
Embodiment 12: take fipronil bisamide 11.0kg and rotenone 6.5kg, then with acrylate homopolymer sodium salt 15.0kg, alkylnaphthalene sulfonate 5.0kg, bentonite 22.0kg, Sodium Polyacrylate 0.2kg, niter cake 0.1kg, diatomite 20.0kg and calcium carbonate 20.2kg.After mixing, through micro jet, be ground into female powder, add again 3.5kg deionized water to mix in female powder, granulation, dry, screening, by the qualified packing of sample analysis, is made the composite water dispersible granules of fipronil bisamide and rotenone.Through check moisture < 2%, lasting foaming characteristic (1min) < 7ml, wetability < 40s, acceleration heat storage stability is qualified.Dilute with water said preparation carries out field control effectiveness test, its 1500 times of liquid to cabbage aphid medication after the control efficiency of the 5th day and 10 days be respectively 90.2% and 92.3%, control efficiency to the 7th day and 14 days after beet armyworm medication is respectively 92.4% and 94.0%, and the control efficiency of the 6th day and 12 days after cotton bollworm medication is respectively to 94.0% and 90.5%.
Embodiment 13: take fipronil bisamide 3.5kg and rotenone 11.0kg, then with acrylate homopolymer sodium salt 5.0kg, alkylphenol polyoxyethylene formaldehyde condensation products 13.0kg, benzyl naphthalene sulfonate 1.5kg, sodium alkyl sulfate 1.0kg, silica gel 15.0kg, dextrin 0.2kg, polyethylene glycol 0.2kg, another name for sodium 0.3kg, niter cake 0.3kg, Emathlite 25.0kg and kaolin 24.0kg.After mixing, through micro jet, be ground into female powder, add again 7.9kg deionized water to mix in female powder, granulation, dry, screening, by the qualified packing of sample analysis, is made the composite water dispersible granules of fipronil bisamide and rotenone.Through check moisture < 2%, lasting foaming characteristic (1min) < 7ml, wetability < 40s, acceleration heat storage stability is qualified.Dilute with water said preparation carries out field control effectiveness test, its 1500 times of liquid to cabbage aphid medication after the control efficiency of the 5th day and 10 days be respectively 95.0% and 93.1%, control efficiency to the 7th day and 14 days after beet armyworm medication is respectively 94.0% and 95.0%, and the control efficiency of the 6th day and 12 days after cotton bollworm medication is respectively to 95.1% and 96.3%.
Embodiment 14: take fipronil bisamide 7.5kg and rotenone 12.0kg, then with acrylate homopolymer sodium salt 15.0kg, alkylnaphthalene sulfonate 5.0kg, bentonite 22.0kg, Sodium Polyacrylate 0.2kg, niter cake 0.1kg, diatomite 20.0kg and calcium carbonate 18.2kg.After mixing, through micro jet, be ground into female powder, add again 6.8kg deionized water to mix in female powder, granulation, dry, screening, by the qualified packing of sample analysis, is made the composite water dispersible granules of fipronil bisamide and rotenone.Through check moisture < 2%, lasting foaming characteristic (1min) < 7ml, wetability < 40s, acceleration heat storage stability is qualified.Dilute with water said preparation carries out field control effectiveness test, its 1500 times of liquid to cabbage aphid medication after the control efficiency of the 5th day and 10 days be respectively 90.9% and 92.7%, control efficiency to the 7th day and 14 days after beet armyworm medication is respectively 92.8% and 94.2%, and the control efficiency of the 6th day and 12 days after cotton bollworm medication is respectively to 94.5% and 91.3%.
Embodiment 15: take fipronil bisamide 16.0kg and rotenone 8.5kg, then with Fluhyzon formaldehyde condensation products 5.0kg, acrylate homopolymer sodium salt 10.0kg, dialkyl group sulfonate 2.5kg, silica gel 15.0kg, dextrin 0.5kg, another name for sodium 0.2kg, kaolin 25.0kg and clay 17.3kg.After mixing, through micro jet, be ground into female powder, add again 5.6kg deionized water to mix in female powder, granulation, dry, screening, by the qualified packing of sample analysis, is made the composite water dispersible granules of fipronil bisamide and rotenone.Through check moisture < 2%, lasting foaming characteristic (1min) < 7ml, wetability < 40s, acceleration heat storage stability is qualified.Dilute with water said preparation carries out field control effectiveness test, its 1500 times of liquid to cabbage aphid medication after the control efficiency of the 5th day and 10 days be respectively 96.2% and 97.3%, control efficiency to the 7th day and 14 days after beet armyworm medication is respectively 97.3% and 98.3%, and the control efficiency of the 6th day and 12 days after cotton bollworm medication is respectively to 96.1% and 97.3%.
Embodiment 16: take fipronil bisamide 1.0kg and rotenone 1.5kg, then with sodium lignin sulfonate 5.0kg, phenethyl phenol polyethenoxy sodium sulphate 4.5kg, acrylate homopolymer sodium salt 5.5kg, alkylnaphthalene sulfonate 1.0kg, sodium alkyl sulfate 1.0kg, benzyl naphthalene sulfonate 2.0kg, ammonium sulfate 8.0kg, bentonite 6.0kg, polyethylene glycol 6.0kg, Sodium Polyacrylate 0.2kg, xanthans 0.1kg, wooden sodium 0.2kg, niter cake 0.1kg, another name for sodium 0.3kg, citric acid 0.1kg, diatomite 10.0kg, clay 14.0kg and kaolin 16.5kg.After mixing, through micro jet, be ground into female powder, add again deionized water to mix in female powder, granulation, dry, screening, by the qualified packing of sample analysis, is made the composite water dispersible granules of fipronil bisamide and rotenone.Through check moisture < 2%, lasting foaming characteristic (1min) < 7ml, wetability < 40s, acceleration heat storage stability is qualified.Dilute with water said preparation carries out field control effectiveness test, its 500 times of liquid to cabbage aphid medication after the control efficiency of the 5th day and 10 days be respectively 93.2% and 95.3%, control efficiency to the 7th day and 14 days after beet armyworm medication is respectively 91.3% and 93.3%, and the control efficiency of the 6th day and 12 days after cotton bollworm medication is respectively to 92.1% and 94.3%.
Embodiment 17: take fipronil bisamide 1.0kg and rotenone 2.5kg, then with alkylbenzenesulfonate 3.0kg, alkylphenol polyoxyethylene formaldehyde condensation products 5.5kg, Fluhyzon formaldehyde condensation products 4.5kg, alkane benzyl naphthalenesulfonate formaldehyde condensation compound 1.0kg, fatty acid amide N methyl taurine salt 2.0kg, dialkyl group naphthalene sulfonate 1.0kg, White Carbon black 7.0kg, bentonite 5.0kg, silica gel 8.0kg, dextrin 0.2kg, sodium carboxymethylcellulose 0.1kg, xanthans 0.2kg, carbonic hydroammonium 0.1kg, another name for sodium 0.3kg, citric acid 0.1kg, acid clay 16.0kg, mica powder 15.0kg and sepiolite 12.5kg.After mixing, through micro jet, be ground into female powder, add again 3.8kg deionized water to mix in female powder, granulation, dry, screening, by the qualified packing of sample analysis, is made the composite water dispersible granules of fipronil bisamide and rotenone.Through check moisture < 2%, lasting foaming characteristic (1min) < 7ml, wetability < 40s, acceleration heat storage stability is qualified.Dilute with water said preparation carries out field control effectiveness test, its 600 times of liquid to cabbage aphid medication after the control efficiency of the 5th day and 10 days be respectively 93.1% and 95.2%, control efficiency to the 7th day and 14 days after beet armyworm medication is respectively 92.3% and 93.9%, and the control efficiency of the 6th day and 12 days after cotton bollworm medication is respectively to 92.7% and 93.9%.
Above-described embodiment shows, the composite water dispersible granules of fipronil bisamide of the present invention and rotenone is not only remarkable to the control efficiency of beet armyworm, cabbage aphid and cotton bollworm, and this water dispersible granules be take water as matrix, overcome the shortcoming of the toxic organic solvent such as cream preparation use dimethylbenzene, particle disintegration rate is fast, there is no bales stained, to environment, people and animals and other beneficial organism safety, be difficult for generation poisoning and insect it is difficult for developing immunity to drugs.Each composition in complex preparation can be worked in coordination with and play a role in application, has made up self deficiency of single dose agricultural chemicals, and has reduced applications of pesticide amount, has reduced the production cost of product.In addition, the cold and hot bin stability of water dispersible granules of the present invention is good, and in use holding effect is permanent, and its preparation technology is simple, and suitability for industrialized is produced and large scale application.