Summary of the invention
The purpose of this invention is to provide a kind of energy and can also protect and bring into play the pesticide preparation-water dispersible granules of piperazine worm pyridine drug effect without organic solvent better; with urea is that not only disintegrating property is better for the water-dispersible granules of main additive; suspensibility is higher; and be that crop has increased nutritive element when using, more can promote the growth of crop.
Another object of the present invention is that the pyridine of piperazine worm, urea, dispersion agent, wetting agent, disintegrating agent, binding agent are stirred under the physical pulverization effect of micronizer mill, it is small solid particulate that each material is pulverized, and adopts the method for wet granulation and extruder grain to make piperazine worm pyridine water dispersible granular preparation.
Purpose of the present invention can reach by following measure:
A kind of paichongding water dispersible granule, form by the component of following weight content:
Piperazine worm pyridine 5%~80% urea 5~25%
Dispersion agent 0.5%~30% wetting agent 1%~10%
Binding agent 0.1%~8% stablizer 0.1%~5%
Disintegrating agent 1%~15% permeate agent 0%~5%
It is 5~7 filler surpluses that the pH value is regulated in the pH regulator agent.
Above-mentioned paichongding water dispersible granule preferably is made up of the component of following weight content:
Piperazine worm pyridine 10%~50% urea 5~25%
Dispersion agent 1%~10% wetting agent 1%~10%
Binding agent 1%~8% stablizer 1%~5%
Disintegrating agent 1%~15% permeate agent 1%~5%
It is 5~7 filler surpluses that the pH value is regulated in the pH regulator agent.
Wetting agent is selected from one or more in sodium lauryl sulphate, Sodium dodecylbenzene sulfonate, sodium laurylsulfate, octylphenol polyethylene oxyethylene group ether sulfate, sulfonated alkyl naphathalene, the alkyl fourth stilbene-4,4'-bis-(1-azo-3, 4-dihydroxy-benzene)-2,2'-disulfonate.
Dispersion agent is selected from sodium lignosulfonate, calcium lignin sulphonate, lauryl alcohol polyethylene glycol oxide base ether sodium sulfate, alkylnaphthalene formaldehyde condensation products iodate, potassium oleate, sodium oleate, the alkyl polyoxyethylene ether iodate, alkylphenol-polyethenoxy base ether formaldehyde condensation products, alkylphenol-polyethenoxy base ether Nonyl pheno base ether, polyoxyethylene polyoxypropylene base ether block copolymers, draw back powder, poly-second carboxylic esters sodium salt, in dodecyl polyoxyethylene ether phosphate or the alkylnaphthalene formaldehyde condensation products vitriol one or more.
Binding agent selects one or more in Macrogol 200~4000, ethylene glycol, propylene glycol, the glycerol.
Stablizer is selected from one or more in pyrocatechol, butylglycidyl ether, phenyl glycidyl ether, cresyl glycidyl ether, polyethylene glycol diglycidylether, Epicholorohydrin, sodium sorbate, epoxidised soybean oil, oleum lini, quinhydrones, Eugenol, citric acid, hydroxy benzoate or the propylparaben.
Disintegrating agent is selected from one or more in salt of wormwood, yellow soda ash, sodium bicarbonate, bicarbonate of ammonia, the ammonium nitrate etc.
One or more permeate agents that the PH conditioning agent is selected from sodium hydroxide, ammoniacal liquor, phosphoric acid ester, citric acid or the phosphoric acid are organosilicon.
Filler is one or more in white carbon black, kaolin, diatomite, the wilkinite.
A kind of method for preparing paichongding water dispersible granule; with the pyridine of piperazine worm, urea, dispersion agent, wetting agent, binding agent, stablizer, disintegrating agent, permeate agent, pH regulator agent and filler behind comminution by gas stream; with wet granulation and Squeezinggranulator, make sphere or columniform particle and get final product.
The present invention has made water dispersible granules with pyridine superfine grinding of piperazine worm and extruder grain, thereby has:
1. the flash-point height does not burn and does not explode, and produces storage and safe in utilization;
2. slaking is good in water, and the suspensibility height has improved the rate of utilization of effective constituent, has reduced dosage;
3. dust is few, and environmental pollution is little, to production and user and environmental safety;
4. without organic solvent, aboundresources is packed easily;
5. the pyridine of piperazine worm had provide protection;
6. after said preparation is sprayed, the crop surface excellent adsorption, the lasting period is long, good disinsection effect; Add urea and can not only strengthen the growth that whole preventive effect more can promote crop;
7. integrated control effect is better after adding permeate agent.
Embodiment
Embodiment 110% paichongding water dispersible granule
Each component concentration (by weight) is piperazine worm pyridine 10%, urea 30%, dispersion agent sodium lignosulfonate 6%, alkylphenol-polyethenoxy base ether formaldehyde condensation products 5%, stablizer pyrocatechol 2%, wetting agent sodium lauryl sulphate 1%, binding agent polyoxyethylene glycol 8005%, disintegrating agent sodium bicarbonate 8%, it is 6 that the PH conditioning agent makes the suspension agent pH value in right amount, permeate agent organosilicon 2%, white carbon black 10%, kaolin is mended to 100%.The pyridine of piperazine worm, dispersion agent, wetting agent, stablizer, disintegrating agent, permeate agent, PH conditioning agent etc. behind comminution by gas stream, with wet granulation and Squeezinggranulator, are made sphere or columniform particle and get final product.
Embodiment 225% paichongding water dispersible granule
Each component concentration (by weight) is piperazine worm pyridine 25%, urea 20%, dispersion agent alkylnaphthalene formaldehyde condensation products iodate 5%, wetting agent sodium laurylsulfate 2%, stablizer butylglycidyl ether 2.5%, binding agent propylene glycol 4%, it is 6 that disintegrating agent yellow soda ash 8%, PH conditioning agent make the suspension agent pH value in right amount, permeate agent organosilicon 2%, white carbon black 15%, kaolin is mended to 100%.Behind comminution by gas stream, with wet granulation and Squeezinggranulator, making sphere or columniform particle can become with the pyridine of piperazine worm, dispersion agent, wetting agent, stablizer, disintegrating agent, permeate agent, PH conditioning agent etc.
Embodiment 340% paichongding water dispersible granule
Each component concentration (by weight) is piperazine worm pyridine 40%, urea 20%, dispersion agent lauryl alcohol polyethylene glycol oxide base ether sodium sulfate 6%, dispersion agent 8%, wetting agent sulfonated alkyl naphathalene 2%, stablizer epoxy soybean oil 2.5%, it is 6 that binding agent glycerol 4%, disintegrating agent ammonium nitrate 10%, PH conditioning agent make the suspension agent pH value in right amount, permeate agent organosilicon 2%, white carbon black is mended to 100%.The pyridine of piperazine worm, dispersion agent, wetting agent, stablizer, disintegrating agent, permeate agent, PH conditioning agent etc. behind comminution by gas stream, with wet granulation and Squeezinggranulator, are made sphere or columniform particle and get final product.
Embodiment 450% paichongding water dispersible granule
Each component concentration (by weight) is piperazine worm pyridine 50%, urea 15%, dispersion agent alkylnaphthalene formaldehyde condensation products carboxylate salt 4%, alkylphenol-polyethenoxy base ether formaldehyde condensation products 5%, wetting agent Sodium dodecylbenzene sulfonate 2%, stablizer phenyl glycidyl ether 2%, binding agent cetomacrogol 1000 5%, disintegrating agent ammonium nitrate 10%, it is 6 that the PH conditioning agent makes the suspension agent pH value in right amount, permeate agent organosilicon 2%, and white carbon black is mended to 100%.The pyridine of piperazine worm, dispersion agent, wetting agent, stablizer, disintegrating agent, permeate agent, PH conditioning agent etc. behind comminution by gas stream, with wet granulation and Squeezinggranulator, are made sphere or columniform particle and get final product.
Embodiment 560% paichongding water dispersible granule
Each component concentration (by weight) is piperazine worm pyridine 60%, dispersion agent lauryl alcohol polyethylene glycol oxide base ether carboxylate 5%, sodium lignosulfonate 3%, wetting agent octylphenol polyethylene oxyethylene group ether sulfate 3%, stablizer phenyl glycidyl ether 2%, binding agent poly(oxyethylene glycol) 400 3%, it is 6 that disintegrating agent salt of wormwood 10%, PH conditioning agent make the suspension agent pH value in right amount, permeate agent organosilicon 2%, white carbon black 1%, urea is mended to 100%.The pyridine of piperazine worm, dispersion agent, wetting agent, stablizer, disintegrating agent, permeate agent, PH conditioning agent etc. behind comminution by gas stream, with wet granulation and Squeezinggranulator, are made sphere or columniform particle and get final product.
Embodiment 670% paichongding water dispersible granule
Each component concentration (by weight) is piperazine worm pyridine 70%, dispersion agent alkylphenol-polyethenoxy base ether formaldehyde condensation products carboxylate salt 5%, alkylnaphthalene formaldehyde condensation products iodate 5%, wetting agent alkyl fourth stilbene-4,4'-bis-(1-azo-3, 4-dihydroxy-benzene)-2,2'-disulfonate 3%, stablizer Eugenol 2%, binding agent poly(oxyethylene glycol) 400 3%, it is 6 that the PH conditioning agent makes the suspension agent pH value in right amount, permeate agent organosilicon 2%, diatomite 2%, sodium bicarbonate 2%, urea is mended to 100%.The pyridine of piperazine worm, dispersion agent, wetting agent, stablizer, disintegrating agent, permeate agent, PH conditioning agent etc. behind comminution by gas stream, with wet granulation and Squeezinggranulator, are made sphere or columniform particle and get final product.
The pyridine of piperazine worm is to the rice hoppers Toxicity Determination
1 test objective
Rice hoppers is an insect pest of rice, have a strong impact on output and the economic benefit of paddy rice, for effectively administering rice hoppers, understand the preventive effect of initiative agricultural chemicals piperazine worm pyridine to water rice hopper, we select representational brown paddy plant hopper to be the control target, in 2008, carried out preventing and treating the Toxicity Determination of rice hoppers in 2009 with paichongding water dispersible granule.
2 test conditionss
2.1 test target
Rice hoppers [Nilaparvata lugens (stal)]: catch adult from field, institute of agricultural sciences experimental plot, Jianhu County, Jiangsu Province.
The rice paddy seed flushing with clean water preferably of will germinateing is floated not plump paddy.24h at normal temperatures soaks seed.Hand-launder seed-grain several times, use 45~50 ℃ warm water washing 1~2 time again, put into plastics casing, cover wet towel, place vernalization in 30 ℃ the constant incubator.When putting into, the plastic tub bottom tilts slightly, makes water not submergence seed-grain as far as possible.Behind the 24h, the rice paddy seed that will show money or valuables one carries unintentionally is spread out in the dish for cultivating equably, does not stack with seed-grain and is advisable.Put the stainless steel rack, place (illumination 2000~3000lx, 16h, 28 ℃ of temperature) cultivation of preserving moisture in the illumination box.Just can be when the rice bud grows up to 1.5cm for laying eggs and raising.
To have the dish for cultivating of rice bud to put into dependent insect cage, fixing, the dependent insect cage back side is to light source.In addition a glass door that is connected to the dependent insect cage of the adult of adopting back from the field is opened, made its Men Yumen relative.Vibrate cage gently, adult is rushed in the cage of new rice bud.Lay eggs 24 or 48h after use the same method again adult removed.The rice bud that adult has been laid eggs is cultivated in the insectary of illumination 12h 27~29 ℃ of room temperatures, keeps the rice bud not cut off the water supply.Behind 6~8d, the ovum hatching.When the rice bud is eaten extremely by planthopper before, must change the rice bud.When changing seedling, earlier cage is inverted gently, is made withered rice bud in the above, put new rice bud into cage again.Behind the 2d, insect is automatically transferred on the rice bud, takes withered rice bud again away.
2.2 plant and instrument
2.2.1 electronic balance (sensibility reciprocal 0.1mg);
2.2.2 clap net;
2.2.3 dependent insect cage (34 * 34 * 34cm
3);
2.2.4 dish for cultivating (28.5 * 28.5 * 0.6cm
3);
2.2.5 the rice bud is rack (26cm * 26cm) fixedly;
2.2.6 micro-dropper;
2.2.7 burn the bosom;
2.2.8 transfer pipet;
2.2.9 constant incubator;
2.2.10 illumination box etc.
3 test design
3.1 the examination material is prepared
Select the nymph in 3 age of the 2nd generation of indoor feeding.
3.2 medicament
(1) Provado (pymetrozine): 95% former medicine;
(2) piperazine worm pyridine (profenofos): 95% former medicine.
Above medicament provides by Kesheng Group Co., Ltd., Jiangsu Prov..
3.3 testing sequence
3.3.1 soup preparation
Earlier with dissolve with ethanol two former medicines, according to the result of preliminary experiment two an amount of former medicines are made into 5 different proportionings, it is stand-by with ethanol each processing to be diluted to the series concentration gradient respectively again.Provado is diluted to 100,50,25,12.5,6.25,3.125mg/L; Piperazine worm pyridine 50,25,12.5,6.25,3.125mg/L are stand-by.
3.3.2 chemicals treatment
The topical application that adopts NY/T 1154.1-2006 to recommend is measured.With micro-dropper solvent cleaning, regulate dropper to stand-by state.Choose the examination worm of neat and consistent with writing brush and use CO
2Slight anesthesia is placed in the 9cm culture dish, then with micro-dropper with medicament by the polypide belly of a drop in the examination worm, every some drops physic liquor 0.1 μ L, with drop 0.1 μ L acetone with contain the tensio-active agent 0.1% tween 80 aqueous solution and be treated to contrast.It is normally to cultivate in 75% the culturing room that examination worm behind the drop is transferred to (28 ± 2) ℃, relative humidity respectively.Every processing 4 times repeats, and whenever repeats to try 20 of worms, 80 of every processing examination worms.
4 investigation
Handle back 24h investigation examination worm death condition (judging that for examination worm death standard be gently to sting no autonomic response with pin), write down total borer population and dead borer population.
5 data statisticss and analysis
5.1 method of calculation
According to enquiry data, calculate the corrected mortality that each is handled, and calculate LC
50If contrast mortality ratio<5% is not proofreaied and correct; The contrast mortality ratio by formula 2 is proofreaied and correct between 5%~20%; Contrast mortality ratio>20%, test need be reformed.
5.2 data statistic analysis
Logarithmic value with drug concentration (mg/L) is independent variable(s) x, is dependent variable y with the probit value of corrected mortality, sets up the virulence regression equation formula respectively, adopts the LC of the single agent of DPS computed in software and each proportioning mixture
50Reach 95% fiducial limit, LC
90And 95% fiducial limit.
6 interpretations of result and discussion
Handle not brown paddy plant hopper nymph in 3 mid-term in age, its LC with the pyridine of piperazine worm
50Value be respectively 10.51 and 20.72mg/L (95% fiducial limit is respectively 8.99~12.33mg/L and 17.80~24.14mg/L), with the LC of contrast medicament Provado
50Value be respectively 17.55 with 42.43mg/L (95% fiducial limit is respectively 15.05~20.94mg/L and compares with 32.71~65.02mg/L), the pyridine of piperazine worm to the virulence of brown paddy plant hopper nymph in 3 age apparently higher than Provado, the former is 1.7 times~2.0 times of the latter, statistical study significant difference (table 1), twice test-results all has same result.Above-mentioned test-results shows that the pyridine of new pesticides piperazine worm has than the better insecticidal activity of Provado brown paddy plant hopper.
The field natural condition are different with indoor conditions, therefore, also there are differences between field population and the indoor population, and can this test-results be further verified by application need under the natural condition of field.
The pyridine of table 1 new pesticides piperazine worm is to the Toxicity Determination result of brown paddy plant hopper
Piperazine worm pyridine field medicine effect test
1, material and method
1.1 reagent agent
1.1.120% red sun agricultural chemicals limited-liability company in Provado SL Nanjing produces, and 25% pyrrole aphid ketone SC Kesheng Group Co., Ltd., Jiangsu Prov. produces
1.1.225% piperazine worm pyridine WG (embodiment 2 gained water dispersible granules)
1.2 Treatment Design
1.2.120% Provado SL 10a.i.g/667m
225% pyrrole aphid ketone SC 5a.i.g/667m
2
1.2.225% piperazine worm pyridine WG 4a.i.g/667m
2
1.2.3 blank (CK)
1.3 using method
Establish 3 processing altogether, each is handled and repeats sub-district area 60m 3 times
2Local rice field four generations brown paddy plant hopper nymph peak period dispenser in 1 age on September 17th, 2009, every 667m
2Press above-mentioned design dosage to water 45kg.Aim at manually evenly complete stool spraying of rice seedling, during dispenser and behind the medicine in the week field keep water layer.
This experimental plot rice varieties is for raising the spoke round-grained rice No. 7.During dispenser, field brown paddy plant hopper hundred cave worms are measured average 4345, wherein 1 age nymph account for 96.4%.
1.4 investigation method
1.4.1 security survey
Sub-district rice seedling growing state is respectively handled in back irregularly observation, and the record rice shoot is analyzed the security of medicament to rice seedling to the reaction or the symptom of chemical damage of medicament.
1.4.2 preventive effect effect research
Before investigation insect population radix, respectively looked into one time the residual worm amount in field behind the medicine in 1,3,7,10,15 day.3 samplings in every sub-district, every some company looks into 6 caves, and 18 caves are looked in every sub-district.Calculate prevention effect with the insect population survival rate, calculation formula is as follows:
Preventive effect (%)=(check plot insect population survival rate-applying area insect population survival rate) ÷ check plot insect population survival rate * 100
2, medicament is to the security of rice seedling
The back is observed, and each sub-district rice seedling growth is normal, any poisoning situation do not occur.
3, result and analysis
25% piperazine worm pyridine WG and 25% pyrrole aphid ketone SC are obvious to paddy rice brown paddy plant hopper preventive effect effect, and 20% Provado is relatively poor to paddy rice brown paddy plant hopper preventive effect, and three kinds of medicaments are all to rice seedling safety, use piperazine worm pyridine WG after the paddy rice growing way be better than other two medicaments.25% pyrrole aphid ketone SC long-lasting is better, and 25% piperazine worm pyridine WG is better on quick-acting.
Table 125% piperazine worm pyridine WG and 25% pyrrole aphid ketone SC, 20% Provado SL
To paddy rice brown paddy plant hopper preventive effect effect
Annotate: A, 25% piperazine worm pyridine WG 4a.i.g/667m
2B, 25% pyrrole aphid ketone SC 5a.i.g/667m
2C, 20% Provado SL 10a.i.g/667m
2