Summary of the invention
The purpose of this invention is to provide a kind of energy and can also protect better and bring into play the pesticidal preparations-water dispersible granules of piperazine worm pyridine drug effect without organic solvent; water-dispersible granules take urea as main additive not only disintegrating property is better; 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, dispersant, wetting agent, disintegrant, binding agent are stirred under the physical crushing effect of airslide disintegrating mill, it is small solid particle 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 measures:
A kind of paichongding water dispersible granule is comprised of the component of following weight content:
Piperazine worm pyridine 5%~80% urea 5~25%
Dispersant 0.5%~30% wetting agent 1%~10%
Binding agent 0.1%~8% stabilizing agent 0.1%~5%
Disintegrant 1%~15% bleeding agent 0%~5%
It is 5~7 filler surpluses that pH adjusting agent is regulated the pH value.
Above-mentioned paichongding water dispersible granule preferably is comprised of the component of following weight content:
Piperazine worm pyridine 10%~50% urea 5~25%
Dispersant 1%~10% wetting agent 1%~10%
Binding agent 1%~8% stabilizing agent 1%~5%
Disintegrant 1%~15% bleeding agent 1%~5%
It is 5~7 filler surpluses that pH adjusting agent is regulated the pH value.
Wetting agent is selected from one or more in lauryl sodium sulfate, neopelex, sldium lauryl sulfate, octylphenol polyethylene oxyethylene group ether sulfate, alkylnaphthalene sulfonate, alkyl fourth disulfonate.
dispersant is selected from sodium lignin sulfonate, calcium lignosulfonate, lauryl alcohol polyethylene glycol oxide base ether sodium sulfate, Fluhyzon formaldehyde condensation products iodate, potassium oleate, enuatrol, 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, pull open powder, poly-second carboxylic esters sodium salt, one or more in alkylpolyoxyethylene phosphate or Fluhyzon formaldehyde condensation products sulphate.
Binding agent selects one or more in Macrogol 200~4000, ethylene glycol, propane diols, glycerine.
Stabilizing agent is selected from one or more in catechol, butyl glycidyl ether, phenyl glycidyl ether, cresyl glycidyl ether, polyethylene glycol diglycidyl ether, chloropropylene oxide, sodium sorbate, epoxidised soybean oil, linseed oil, quinhydrones, eugenol, citric acid, hydroxy benzoate or nipasol.
Disintegrant is selected from one or more in potash, sodium carbonate, sodium bicarbonate, carbonic hydroammonium, ammonium nitrate etc.
One or more bleeding agents that the PH conditioning agent is selected from sodium hydroxide, ammoniacal liquor, phosphate, citric acid or phosphoric acid are organosilicon.
Filler is one or more in white carbon, kaolin, diatomite, bentonite.
A kind of method for preparing paichongding water dispersible granule; with the pyridine of piperazine worm, urea, dispersant, wetting agent, binding agent, stabilizing agent, disintegrant, bleeding agent, pH adjusting agent and filler after air-flow crushing; with wet granulation and Squeezinggranulator, make spherical or columniform particle and get final product.
The present invention has made water dispersible granules with the pyridine ultra-fine grinding of piperazine worm and extruder grain, thereby has:
1. flash-point is high, does not burn and does not explode, and produces and stores and use safety;
2. disintegrative is good in water, and suspensibility is high, has improved the utilization rate of active ingredient, has reduced dosage;
3. dust is few, and environmental pollution is little, to production and user and Environmental security;
4. without organic solvent, aboundresources is easily packed;
5. the pyridine of piperazine worm had protective effect;
6. after said preparation is sprayed, the crop surface excellent adsorption, the lasting period is long, good disinsection effect; Add urea can not only strengthen whole preventive effect and more can promote the growth of crop;
7. after adding bleeding agent, integrated control effect is better.
Embodiment
Embodiment 110% paichongding water dispersible granule
Each constituent content (by weight) is piperazine worm pyridine 10%, urea 30%, dispersant sodium lignin sulfonate 6%, alkylphenol-polyethenoxy base ether formaldehyde condensation products 5%, stabilizing agent Catechol 2 %, wetting agent lauryl sodium sulfate 1%, binding agent polyethylene glycol 8005%, disintegrant sodium bicarbonate 8%, it is 6 that the PH conditioning agent makes the suspending agent pH value in right amount, bleeding agent organosilicon 2%, white carbon 10%, kaolin is mended to 100%.The pyridine of piperazine worm, dispersant, wetting agent, stabilizing agent, disintegrant, bleeding agent, PH conditioning agent etc. after air-flow crushing, with wet granulation and Squeezinggranulator, are made spherical or columniform particle and get final product.
Embodiment 225% paichongding water dispersible granule
Each constituent content (by weight) is piperazine worm pyridine 25%, urea 20%, dispersant Fluhyzon formaldehyde condensation products iodate 5%, wetting agent sldium lauryl sulfate 2%, stabilizing agent butyl glycidyl ether 2.5%, binding agent propane diols 4%, it is 6 that disintegrant sodium carbonate 8%, PH conditioning agent make the suspending agent pH value in right amount, bleeding agent organosilicon 2%, white carbon 15%, kaolin is mended to 100%.After air-flow crushing, with wet granulation and Squeezinggranulator, making spherical or columniform particle can become with the pyridine of piperazine worm, dispersant, wetting agent, stabilizing agent, disintegrant, bleeding agent, PH conditioning agent etc.
Embodiment 340% paichongding water dispersible granule
Each constituent content (by weight) is piperazine worm pyridine 40%, urea 20%, dispersant lauryl alcohol polyethylene glycol oxide base ether sodium sulfate 6%, dispersant 8%, wetting agent alkylnaphthalene sulfonate 2%, stabilizing agent epoxidized soybean oil 2.5%, it is 6 that binding agent glycerine 4%, disintegrant ammonium nitrate 10%, PH conditioning agent make the suspending agent pH value in right amount, bleeding agent organosilicon 2%, white carbon is mended to 100%.The pyridine of piperazine worm, dispersant, wetting agent, stabilizing agent, disintegrant, bleeding agent, PH conditioning agent etc. after air-flow crushing, with wet granulation and Squeezinggranulator, are made spherical or columniform particle and get final product.
Embodiment 450% paichongding water dispersible granule
Each constituent content (by weight) is piperazine worm pyridine 50%, urea 15%, dispersant Fluhyzon formaldehyde condensation products carboxylate 4%, alkylphenol-polyethenoxy base ether formaldehyde condensation products 5%, wetting agent neopelex 2%, stabilizing agent phenyl glycidyl ether 2%, binding agent cetomacrogol 1000 5%, disintegrant ammonium nitrate 10%, it is 6 that the PH conditioning agent makes the suspending agent pH value in right amount, bleeding agent organosilicon 2%, and white carbon is mended to 100%.The pyridine of piperazine worm, dispersant, wetting agent, stabilizing agent, disintegrant, bleeding agent, PH conditioning agent etc. after air-flow crushing, with wet granulation and Squeezinggranulator, are made spherical or columniform particle and get final product.
Embodiment 560% paichongding water dispersible granule
Each constituent content (by weight) is piperazine worm pyridine 60%, dispersant lauryl alcohol polyethylene glycol oxide base ether carboxylate 5%, sodium lignin sulfonate 3%, wetting agent octylphenol polyethylene oxyethylene group ether sulfate 3%, stabilizing agent phenyl glycidyl ether 2%, binding agent PEG400 3%, it is 6 that disintegrant potash 10%, PH conditioning agent make the suspending agent pH value in right amount, bleeding agent organosilicon 2%, white carbon 1%, urea is mended to 100%.The pyridine of piperazine worm, dispersant, wetting agent, stabilizing agent, disintegrant, bleeding agent, PH conditioning agent etc. after air-flow crushing, with wet granulation and Squeezinggranulator, are made spherical or columniform particle and get final product.
Embodiment 670% paichongding water dispersible granule
Each constituent content (by weight) is piperazine worm pyridine 70%, dispersant alkylphenol-polyethenoxy base ether formaldehyde condensation products carboxylate 5%, Fluhyzon formaldehyde condensation products iodate 5%, wetting agent alkyl fourth disulfonate 3%, it is 6 that stabilizing agent eugenol 2%, binding agent PEG400 3%, PH conditioning agent make the suspending agent pH value in right amount, bleeding agent organosilicon 2%, diatomite 2%, sodium bicarbonate 2%, urea is mended to 100%.The pyridine of piperazine worm, dispersant, wetting agent, stabilizing agent, disintegrant, bleeding agent, PH conditioning agent etc. after air-flow crushing, with wet granulation and Squeezinggranulator, are made spherical 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 the primary pest of paddy rice, have a strong impact on output and the economic benefit of paddy rice, for effectively administering rice hoppers, understand the pyridine of initiative agricultural chemicals piperazine worm to the preventive effect of water rice hopper, we select representational brown planthopper 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 experimental conditions
2.1 test target
Rice hoppers [Nilaparvata lugens (stal)]: catch adult from field, institute of agricultural sciences experimental field, Jianhu County, Jiangsu Province.
To germinate preferably that rice paddy seed rinses with clear water, float not plump paddy.24h at normal temperatures soaks seed.Hand-launder seed-grain several times, then use the warm water washing 1~2 time of 45~50 ℃, put into plastic casing, cover wet towel, be placed in vernalization in the constant incubator of 30 ℃.When putting into, the inclination slightly of plastic basin bottom makes water not submergence seed-grain as far as possible.After 24h, the rice paddy seed that will show money or valuables one carries unintentionally is spread out in dish for cultivating equably, does not stack with seed-grain and is advisable.Put Stainless-steel space grids, be placed in (illumination 2000~3000lx, 16h, 28 ℃ of temperature) water-retaining cultivation in illumination box.Just can be for laying eggs and raising when the rice bud grows up to 1.5cm.
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.Separately 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 gently cage, 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.After 6~8d, the ovum hatching.Eaten extremely by rice fulgorid when the rice bud before, must change the rice bud.When changing seedling, first cage is inverted gently, is made withered rice bud in the above, then put new rice bud into cage.After 2d, insect is automatically transferred on the rice bud, then takes withered rice bud away.
2.2 instrument and equipment
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 intravenous drip device;
2.2.7 burn the bosom;
2.2.8 pipette;
2.2.9 constant incubator;
2.2.10 illumination box etc.
3 experimental scheme
3.1 the examination material is prepared
Select the 2nd generation nymph in 3 age of indoor feeding.
3.2 medicament
(1) Imidacloprid (pymetrozine): 95% former medicine;
(2) piperazine worm pyridine (profenofos): 95% former medicine.
Above medicament provides by Kesheng Group Co., Ltd., Jiangsu Prov..
3.3 test procedure
3.3.1 liquid preparation
First with ethanol dissolving two former medicines, according to the result of preliminary experiment, two appropriate former medicines are made into 5 different proportionings, then it is stand-by with ethanol, each processing to be diluted to respectively the series concentration gradient.Imidacloprid 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 drop method that adopts NY/T 1154.1-2006 to recommend is measured.With micro intravenous drip device solvent clean, regulate dropper to stand-by state.Choose the examination worm CO of neat and consistent with writing brush
2Slight anesthesia is placed in the 9cm culture dish, then with the micro intravenous drip device with medicament by the polypide belly of a drop in the examination worm, every some drops physic liquor 0.1 μ L is with drop 0.1 μ L acetone with contain the surfactant 0.1% Tween 80 aqueous solution and be treated to contrast.It is normally to cultivate in 75% culturing room that examination worm after drop is transferred to respectively (28 ± 2) ℃, relative moisture.Every processing 4 times repeats, and often repeats to try 20 of worms, 80 of every processing examination worms.
4 investigation
After processing, 24h investigation examination worm death condition (judgement is gently to sting without autonomic response with pin for examination worm death standard), record total borer population and dead borer population.
5 data statistics and analysis
5.1 computational methods
According to survey data, calculate the corrected mortality that each is processed, and calculate LC
50If contrast lethality<5% is not proofreaied and correct; The contrast lethality by formula 2 is proofreaied and correct between 5%~20%; Contrast lethality>20%, test need be reformed.
5.2 data statistic analysis
Take the logarithm value of drug concentration (mg/L) as independent variable x, take the probit value of corrected mortality as dependent variable y, set up respectively the virulence regression equation formula, adopt DPS software to calculate the LC of single dose and each proportioning mixture
50Reach 95% confidence limit, LC
90And 95% confidence limit.
6 interpretations of result and discussion
Process not brown planthopper 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% confidence limit is respectively 8.99~12.33mg/L and 17.80~24.14mg/L), with the LC of contrast medicament Imidacloprid
50Value is respectively 17.55, and (95% confidence limit is respectively 15.05~20.94mg/L and compares with 32.71~65.02mg/L) with 42.43mg/L, the pyridine of piperazine worm to the virulence of brown planthopper nymph in 3 age apparently higher than Imidacloprid, the former is 1.7 times~2.0 times of the latter, statistical analysis significant difference (table 1), twice result of the test all has same result.Above-mentioned result of the test shows that the pyridine of new pesticides piperazine worm has than the better insecticidal activity of Imidacloprid brown planthopper.
The field natural conditions are different from indoor conditions, therefore, also there are differences between field population and indoor population, and under the natural conditions of field, can this result of the test be used needs further checking.
The Toxicity Determination result of table 1 new pesticides piperazine worm pyridine to brown planthopper
Piperazine worm pyridine field medicine effect test
1, material and method
1.1 reagent agent
1.1.120% Imidacloprid SL Nanjing red sun agricultural chemicals limited company produces, and 25% pymetrozine 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% Imidacloprid SL 10a.i.g/667m
225% pymetrozine 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 altogether 3 processing, each is processed and repeats 3 times, residential quarter area 60m
2Local rice field four generations brown planthopper nymph in 1 age peak period dispenser 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 after medicine in the week field keep water layer.
This experimental field rice varieties is for raising the spoke round-grained rice No. 7.During dispenser, average 4345 of field brown planthopper hundred cave worm amount, wherein 1 age nymph account for 96.4%.
1.4 investigation method
1.4.1 security survey
Residential quarter rice seedling growing state is respectively processed in rear irregularly observation, and reaction or the symptom of chemical damage of record rice shoot to medicament analyzed medicament to the safety of rice seedling.
1.4.2 preventive effect effect research
Front investigation insect population radix was respectively looked into one time the residual worm amount in field in 1,3,7,10,15 day after medicine.The sampling of 3 of every residential quarters, every some company looks into 6 caves, and 18 caves are looked in every residential quarter.Calculate control efficiency with the insect population survival rate, computing 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, the safety of medicament to rice seedling
Rear observation, each residential quarter rice seedling growth is normal, any poisoning situation do not occur.
3, results and analysis
25% piperazine worm pyridine WG and 25% pymetrozine SC are to Brown Planthopper preventive effect successful, and 20% Imidacloprid is relatively poor to the Brown Planthopper 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% pymetrozine SC lasting effect is better, and 25% piperazine worm pyridine WG is better on quick-acting.
Table 125% piperazine worm pyridine WG and 25% pymetrozine SC, 20% Imidacloprid SL
To Brown Planthopper preventive effect effect
Annotate: A, 25% piperazine worm pyridine WG 4a.i.g/667m
2B, 25% pymetrozine SC 5a.i.g/667m
2C, 20% Imidacloprid SL 10a.i.g/667m
2