CN101011051B - Water dispersion granule for disinsection - Google Patents
Water dispersion granule for disinsection Download PDFInfo
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- CN101011051B CN101011051B CN200610011311A CN200610011311A CN101011051B CN 101011051 B CN101011051 B CN 101011051B CN 200610011311 A CN200610011311 A CN 200610011311A CN 200610011311 A CN200610011311 A CN 200610011311A CN 101011051 B CN101011051 B CN 101011051B
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Abstract
The invention relates to a water-dispersible particle which can be used in disinfection. The invention is prepared from following components that 0.4-10 deals of cnidium fruit extractive, 2-20 deals of mixture solvents, 1.5-15 deals of mixture emulsifier, 4-15 deals of mixture lagging cover, and 40-90 deals of corn material. The inventive production is based one multiply adsorptions and lagging technique, while it can disinfect and adjust the growth, with little organic solvent.
Description
Technical field
The present invention relates to pesticide field, more particularly, relate to a kind of water dispersion granule of novel pesticide-germicide.
Background technology
To be the Chinese herbal medicine frutus cnidii carry or hot reflux extracts to concentrate behind alcohol soluble substance or the molten thing of ester and forms through the organic solvent cold soaking common cnidium fruit P.E, and also available carbonic acid gas critical point extraction extracts and forms.Mainly contain Osthole in common cnidium fruit P.E, several have bioactive compound also to contain xanthotoxin, citrene, cnidiadin etc. simultaneously.Existing a large amount of experimental datas proof common cnidium fruit P.Es and Osthole have strong antifungic action, and protozoas such as the tens kinds of insect larvaes of Lepidoptera, Homoptera, diptera, coleoptera and trichomonad are had stronger killing action.Therefore, common cnidium fruit P.E and Osthole are registered as agricultural insecticide and agricultural fungicidal agent in China.The cnidium monnieri subclass pesticidal preparations of having registered comprises missible oil, two kinds of formulations of aqueous emulsion, and Shang Weijian has other formulation registration and report of Osthole and frutus cnidii pesticide-germicide agricultural chemicals.
The production technology of the water dispersion granule of general agricultural chemicals is divided into one-shot forming and post forming two classes.The first kind is to utilize large-scale granulation tower that material is sprayed dried forming, and product particle is very little, and equipment investment is very big, and property is good but product moisture looses.Second class is the way granulation by extruding, and the dry powder or the slurry extruding slivering of promptly earlier material being made certain fineness cut into grain, perhaps directly are squeezed into granule, and product particle is suitable, but the aqueous dispersion performance is relatively poor.Relevant patent (the Chinese patent application 200410009966.8 of application such as professor Xie Jiugao, 20051011428.7, patent ZL02131126.9, and patent application PCT/CN2005/001600) then is the water dispersion granule that the Avermectin, methylamino avermectin, the Avermectin that adopt the absorption coating method to produce three-layer structure adds product such as efficient cypermethrin compounded.This new technology equipment is simple, invests seldom, and the production time significantly shortens, and product granularity is moderate, and water dispersible is good.And consumption of organic solvent seldom, eliminated the poisoning of organic solvent to environment substantially.In order to adapt to the particularity of common cnidium fruit P.E, the present invention adopts professor's Xie Jiugao etc. absorption art for coating, and will adsorb coating method and be divided into and once adsorb dressing and multiple adsorb and coating method repeatedly, produces the brand-new formulation of cnidium monnieri subclass agricultural chemicals.
Summary of the invention
(1) technical problem that will solve
Purpose of the present invention be intended to a kind of good drug efficacy, cost low, pollute the little pesticide-germicide water dispersion granule that contains common cnidium fruit P.E, another object of the present invention provides the preparation method of this granule.
(2) technical scheme
The water dispersion granule of pesticide-germicide provided by the invention be by by weight or the following raw materials according of volume proportion prepare: in common cnidium fruit P.E 0.4-10 part of Osthole content, other pesticide-germicide materials 0-20 part, mixed solvent 2-20 part, blended emulsifier 1.5-15 part is mixed seed coating medicine 4-15 part and core 40-90 part.
The above common cnidium fruit P.E is with carbonic acid gas critical point extraction, extracting pressure: 15-25MPa wherein, temperature: 35-45 ℃, separation reactor I pressure: 5-15MPa, temperature: 45-65 ℃; Separation reactor I I pressure: 5-10MPa, temperature: 55-65 ℃; CO
2Flow: 75L-150L/Hr. (5 liters of devices), extraction time: 40 minutes-2 hours.
Perhaps paste mixture or the powder mixture that obtains with other conventional extracting method; Conventional extracting method has ethanol or ethyl acetate cold soaking (ZL01136788.1), alcohol reflux (basic unit's Chinese medicine magazine, 2000,14 (1): 47) two kinds, in the extract except that Osthole, also having compositions such as Imperatorin, xanthotoxin. extract all is that the content in Osthole comes, the content of Osthole is measured with the HPLC method, and the chromatographic column filler is Hypersil C
18, 5 μ are flowing phase with methyl alcohol+water=80+20, detect wavelength 322nm.
Describedly be used for other composite pesticide-germicide materials and be selected from Avermectin or derivatives thereof, pleocidin, pyrethroid insecticides, urea insecticide, organophosphorus insecticides, one or more in generation height, lucky star, tpn, phonetic mould amine, Polyoxin, the Buddhist nun's Mycosporin;
Described mixed solvent is selected from the 2-4 kind in methyl alcohol, ethanol, ethyl acetate, monochloro methane, carrene, dimethyl sulfoxide (DMSO) and the acetone.
Described blended emulsifier is selected from two kinds in Tx-10 (being polyoxyethylene nonylphenol ether EO-9.5, mean molecule quantity 616), polysorbate40, polysorbate60, Tween 80, anionic dodecyl sodium sulfate and the calcium dodecyl benzene sulfonate;
Described mixing seed coating medicine is selected from the material of non-activities such as white carbon black, diatomite, kaolin, cellulose powder, soluble starch, dextrin, dodecyl sodium sulfate, also can from Powdered agricultural chemicals such as following several materials that bactericidal and insecticidal activity arranged such as bacillus thuringiensis,Bt bacterium powder, Buddhist nun's Mycosporin, compound sodium nitrophenolate, Acetamiprid, choose, form with the 2-4 kind in the above-mentioned substance and mix seed coating medicine;
Described core is selected from urea, boron fertilizer, KCl, sucrose, NH
4H
2PO
4,, C
uSO
4, and one or more compositions in active substance compound sodium nitrophenolate (little granular) and the generation height (little granular) mix core.Select according to Different Crop and controlling object, for example, can select sucrose when controlling object during for insect is core; When controlling object can be selected the core that mixes that urea and compound sodium nitrophenolate form during for plant pathogenic fungi; It is core that the special-purpose agricultural chemicals of rape is selected the boron fertilizer particle; It is core that the special-purpose agricultural chemicals of leaf vegetables is selected urea; Whether avoid chlorion according to crop, whether need to replenish situations such as phosphate fertilizer, can also select KCl or phosphorus ammonium is core.
Composite granule comprises the composite of Osthole and insecticide among the present invention, the composite and Osthole of Osthole and bactericide and plant growth regulator composite.Activated species in composite and preferred proportion scope see Table 1.
The preferable compound proportion scope and the synergistic effect of table 1 fructus cnidii complex granule
| Active substance A | Active substance B | A∶B(w/w) | CTC value scope | Purposes |
| Osthole | Bacillus thuringiensis bacterium powder (50000IU/mg) (Bacillus. thuringinesis.aizawai) | 1∶(0.1-6) | ≥120 | Kill the lepidoptera pest larva |
| Osthole | Buddhist nun's Mycosporin (Nikkomycia) | 1∶(2-100) | ≥130 | The powdery mildew Alternaria alternate |
| Osthole | 10% generation height | 1∶(0.2-5) | ≥130 | Banded sclerotial blight false smut alternaria leaf spot of apple |
| Active substance A | Active substance B | A∶B(w/w) | CTC value scope | Purposes |
| Osthole | Acetamiprid | 1∶(0.5-10) | ≥140 | Vegetable aphid |
| Osthole | Avermectin | 1∶(0.5-5) | ≥140 | The diamond-back moth cabbage caterpillar |
| Osthole | Compound sodium nitrophenolate | 1∶(0.01-1) | - | The powdery mildew gray mold |
| Osthole | Sharp strength spy | 1∶(1-10) | ≥150 | The diamond-back moth snout moth's larva of rice |
| Osthole | Cyhalothrin | 1∶(0.2-2.5) | ≥150 | The diamond-back moth snout moth's larva of rice |
| Osthole | Tpn | 1∶(1-20) | ≥130 | White powder, downy mildew |
Common cnidium fruit P.E water dispersion granule of the present invention prepares by following step:
(1) pulverizing that mixes seed coating medicine with mix: be crushed to more than 325 orders after mixing various compositions (except the white carbon black) mixing of seed coating medicine,, other seed coating medicine powder and the white carbon black that crushes mixed if contain white carbon black in the seed coating medicine;
(2) preparation of mixed solvent;
(3) dissolving of active substance with mix: dissolve common cnidium fruit P.E and other composite active substances respectively with mixed solvent, again with the two solution mixing;
(4) blended emulsifier and active substance mixed solution are fully mixed;
(5) under agitation step (4) gained compound is evenly sprayed to the core surface;
(6) under agitation will mix the particle surface that seed coating medicine is sprayed to step (5) gained, continue stir about 12-18 minute after the been sprayed.
(3) beneficial effect
Common cnidium fruit P.E pesticide-germicide water dispersion granule of the present invention is compared following advantage with existing frutus cnidii insecticides: the consumption that 1, significantly reduces organic solvent, and it is inflammable and explosive without dimethylbenzene, toluene etc., the solvent that environment is had adverse effect, make more environmental protection of product, production process is safer; 2, solid pharmaceutical preparation requires to be lower than liquid preparation to packaging material, and the price that adds the solid core is well below organic solvent, and the cost of final preparation can have significantly reduction than original preparation; 3, suitable core is selected and compatibility, can promote the common cnidium fruit P.E original activity, and product desinsection, sterilization, three kinds of functions of growth promotion are had both.
Embodiment
Embodiment 1
Core is selected for use: the high-dispersed granule 750kg of 10% generation;
Blended emulsifier is: the Tx-10 of equivalent and calcium dodecyl benzene sulfonate, the two common 75kg, fully mixing;
Mixed solvent is: ethyl acetate 70% and methyl alcohol 30%, the two common 25L;
Mixing seed coating medicine is: dodecyl sodium sulfate 20%, and rare earth fertilizer powder 20%, white carbon black (325 orders, expanded mistake) 60%, the three is 105kg altogether, and the two kinds of compositions in front require to be crushed to more than 325 orders with airslide disintegrating mill earlier, and are standby with white carbon black mixing then.
Take by weighing Osthole content and be 20% common cnidium fruit P.E medicinal extract 51kg and mixed solvent, blended emulsifier and successively drop into blend tank, start agitator, stir the slurry (medicine curtain material) that obtains homogeneous transparent half an hour;
The agent of generation high-moisture scattered seed is dropped in the comminutor, start comminutor and stir.By spray equipment the medicine curtain carefully is sprayed on the high particle surface of generation immediately, the range request of crossing of whole spray medicine curtain constantly stirs speed of agitator 40-80 rev/min;
To mix seed coating medicine and seed coating medicine evenly be spilt into comminutor, stir, and speed of agitator 40-50 rev/min, make the granule surface all be surrounded by uniform seed coating medicine while spilling by the powder device.
Present embodiment produces product 1000kg, after testing, contains Osthole 1.01% in the granule, and 7.50%, two kind of effective ingredient of the effective ingredient that generation is high (Difenoconazole) adds up to 8.51%.
Embodiment 2
Core is selected for use: urea crystal 720kg;
Blended emulsifier is: Tween 80 75% and calcium dodecyl benzene sulfonate 25%, the two common 30kg, fully mixing;
Mixed solvent is: cyclohexanone 40%, absolute ethyl alcohol 60%, the two common 50L;
Mixing seed coating medicine is: neopelex 20%, soluble starch 30%, white carbon black 50%, the three is 45kg altogether, three's mixing after airslide disintegrating mill to be crushed to 325 orders standby.
Take by weighing Osthole content and be 30% former powder 34.2kg, add mixed solvent, blended emulsifier, the three stirs in blend tank, adds 100 kilograms in the former powder of Bt16000/mg, and fully mixing obtains medicine curtain material.
Urea granules is dropped in the comminutor, start agitator.With spray equipment medicine curtain material carefully is sprayed at the urea granules surface while stirring.Speed of agitator 80-120 rev/min.After waiting to stir, sprayed medicine curtain thing and spread mixing seed coating medicine 45kg again.Be stirred well to evenly.
Present embodiment produces water dispersion granule 979.2kg, contains Osthole 1.05% after testing in the granule, the crystal proteins 0.7% of bacillus thuringiensis,Bt, and effective ingredient adds up to 1.75%.
Embodiment 3
Core is selected for use: urea granules 700kg;
Blended emulsifier is: polysorbate60 80%, calcium dodecyl benzene sulfonate 20%, the two common 20kg, fully mixing.
Mixed solvent is: carrene and methyl alcohol (1: 1 volume) are formed, the two common 150L.
Mixing seed coating medicine is: dodecyl sodium sulfate 20%, and soluble starch 30%, white carbon black 50%, the three is 220kg altogether, and the former two is crushed to 325 orders through airslide disintegrating mill, fully mixes standby with white carbon black again.
Take by weighing 30% Osthole 68kg, add mixed solvent, blended emulsifier, the three stirs in blend tank, obtains medicine curtain material 238kg;
Urea granules is dropped in the comminutor, start agitator.With spray equipment medicine curtain material carefully is sprayed on the surface of urea granules speed of agitator 60-80 rev/min while stirring.Stirred again 5 minutes after having sprayed the medicine curtain, the medicine curtain is adsorbed on the urea granules surface equably.And then spread the mixing seed coating medicine, spread while stirring, spread seed coating medicine after, directly stir to whole particle surface evenly.
Present embodiment produces common cnidium fruit P.E water dispersion granule 1158kg, contains Osthole 1.8% in the granule product after testing.
Embodiment 4
Core is selected for use: the granule 640kg of instant boron fertilizer;
Blended emulsifier is: Tx-10 60%, calcium dodecyl benzene sulfonate 40%, the two common 50kg, fully mixing;
Mixed solvent is: ethyl acetate 60%, methyl alcohol 40%, the two common 60L;
Mixing seed coating medicine is: Buddhist nun's Mycosporin powder 50% that dodecyl sodium sulfate 25%, 20 ten thousand is tired, and lactose 25%, the three is 130kg altogether, and it is standby to be crushed to 325 orders by airslide disintegrating mill behind the mixing.
Take by weighing 50% Osthole bulk drug 120kg, add mixed solvent, blended emulsifier is stirred to the syrupy shape medicine curtain that is dissolved as homogeneous transparent at blend tank;
Instant boron fertilizer particle is dropped in the comminutor, start agitator.Speed of agitator 60-80 rev/min.Spray medicine curtain and seed coating medicine equably.Divide 4 sprayings, spray medicine curtain 57.5kg for the first time, spread seed coating medicine 33kg, spray medicine curtain 57.5kg again, spread seed coating medicine 33kg, so repeat totally four times, sprayed whole medicine curtains and seed coating medicine, finish granulation work.
Present embodiment is produced common cnidium fruit P.E water dispersion granule 998.5kg, and the content of Osthole is 6.01% in the granule after testing.
Embodiment 5
Core is selected for use: white granulated sugar crystal 6 40kg;
The blended emulsifier proportioning is total to 100kg with embodiment 4;
The mixed solvent proportioning is total to 50L with embodiment 4;
Mixing seed coating medicine is: neopelex 20%, and glucose 40%, diatomite 5%, white carbon black 35%, four is 160kg altogether, earlier the front three is mixed the back and is crushed to 320 orders with airslide disintegrating mill, and is standby with the abundant mixing of white carbon black then.
Take by weighing 80% Osthole bulk drug 100kg, add mixed solvent, blended emulsifier is stirred to the syrupy shape medicine curtain that is dissolved as homogeneous transparent at blend tank, and is standby;
Take by weighing white granulated sugar crystal 6 40kg, drop in the comminutor, start agitator, speed of agitator 60-80 rev/min, with reference to embodiment 4 spraying medicine curtain and seed coating medicines, spraying and dressing are 5 times repeatedly.The each medicine of spraying earlier curtain material 50kg spreads and mixes seed coating medicine 32kg.5 shared medicine curtain amount 250kg spread and mix seed coating medicine 160kg.
Present embodiment produces common cnidium fruit P.E water dispersion granule 1001.5kg, contains Osthole 8.0% after testing in the granule.
Embodiment 6
Core is selected for use: anhydrous potassium sulfate is total to 800kg with the core that mixes that urea (3: 5 weight) is formed;
Blended emulsifier is: polysorbate60 80%, and farming breast No. 500 20%, the two common 20kg fully mixes;
Mixed solvent is: methyl alcohol 50%, ethyl acetate 50%, the two common 90L;
Mixing seed coating medicine is: neopelex 20%, and soluble starch 30%, white carbon black 50%, the three is 200kg altogether, fully mixes standby with starch, white carbon black neopelex after airslide disintegrating mill is crushed to 325 orders earlier.
Take by weighing content and be 50% frutus cnidii bulk drug 34kg, the former medicine 25kg of 95% cyhalothrin with the mixed solvent dissolving, adds blended emulsifier, stirs in preparing tank, and is standby.
To mix core and drop in the comminutor, start agitator.Speed of agitator 60-80 rev/min.
Method spraying medicine curtain and seed coating medicine with reference to embodiment 3.
Present embodiment produces common cnidium fruit P.E water dispersion granule 1169kg, contains Osthole 1.45% after testing in the granule, and cyhalothrin 2.03%, effective ingredient total content are 3.48%.
Embodiment 7
Core is selected for use: urea 700kg;
Blended emulsifier is: Tween 80 75%, farming breast No. 500 25%, the two common 32kg, fully mixing;
Mixed solvent is: carrene 40%, acetone 60%, the two common 60L;
Mixing seed coating medicine is: neopelex 20%, and soluble starch 30%, white carbon black 50%, the three is 150kg altogether, fully mixes standby with reference to embodiment 6.
Take by weighing content and be 30% Osthole bulk drug 69kg, the special former medicine 24kg of 95% sharp strength adds mixed solvent and stirs and make two kinds of medicine dissolutions, adds blended emulsifier again, stirs.
Urea granules is dropped in the comminutor reference example 3 methods spraying medicine curtain and seed coating medicine.
Present embodiment produces the sharp water dispersion granule 1033.4kg of snake, contains Osthole 2.0% after testing in the product, sharp strength spy 2.01%.
Embodiment 8
Core is selected for use: urea granules is formed with sucrose (4: 3 weight) and is mixed core 700kg altogether.
Blended emulsifier is: polysorbate60 80%, calcium dodecyl benzene sulfonate 20%, the two common 20kg, fully mixing;
Mixed solvent is: acetone and isopropyl alcohol (4: 3 volumes) are formed mixed solvent, the two common 70L.
Mixing seed coating medicine is: neopelex 20%, and soluble starch 30%, white carbon black 50%, the three is 90kg altogether, and the former two is crushed to 325 orders with airslide disintegrating mill, and is standby with the abundant mixing of white carbon black again.
Take by weighing the former powder 21kg of 95.5% Avermectin, add mixed solvent, stir, treat that Avermectin is dissolved substantially after, and then to add content be 30% Osthole bulk drug 34kg, continues to stir, and adds blended emulsifier after about 10 minutes.Fully stir, uniform medicine curtain is standby until forming.
To mix core and drop into comminutor, start agitator, speed of agitator 60-80 rev/min, by example 3 methods spraying medicine curtain material and seed coating medicine.
Present embodiment is produced snake Ah water dispersion granule 935kg, contains Osthole 1.09% after testing in the product.Avermectin (B
1) 2.14%.
Embodiment 9
Core is selected for use: urea, CuSO
4Be total to 670kg with KCl (8: 1: 1 weight);
Blended emulsifier is: Tx-10 75%, calcium dodecyl benzene sulfonate 25%, the two common 80kg, fully mixing;
Mixed solvent is: methyl alcohol 50%, and ethyl acetate 40%, dimethyl sulfoxide (DMSO) 10%, the three is 80L altogether;
Mixing seed coating medicine is: neopelex 25%, and white carbon black 75%, the two common 180kg, the former is crushed to, and the abundant mixing of carbon black is standby behind 325 orders and in vain.
Take by weighing effective content 90% above Polyoxin raw material 30kg,, cross colloid mill, wear into the thin pulp shape, add the common cnidium fruit P.E 40kg of Osthole content 50% again, stir, if irregular then after a colloid mill with the outstanding turbid shape of mixed solvent furnishing.Add blended emulsifier at last, fully stir until forming translucent medicine curtain material.
Weighing core materials 670kg, the comminutor of packing into starts agitator, speed of agitator 40-60 rev/min.Spray repeatedly and dressing, process is with embodiment 4.Each spray medicine curtain material 46kg sprays 5 times, sprays medicine curtain material 230kg altogether, and preceding 4 dressings spread seed coating medicine 30kg at every turn, spread seed coating medicine 60kg for the last time, shared mixing seed coating medicine 180kg.
Present embodiment is produced snake oxygen water dispersion granule 1080kg, contains Osthole 1.85% after testing in the product.Polyoxin 2.5%.
Embodiment 10
Core is selected for use: present embodiment is selected C for use
uSO
42H
2O crystallization 620kg;
Blended emulsifier is: Tx-10 50%, farming breast No. 100 50%, the two common 80kg, fully mixing;
Mixed solvent is: methyl alcohol 65%, and ethyl acetate 30%, dimethyl sulfoxide (DMSO) 5%, the three is 80L altogether;
Mixing seed coating medicine is: neopelex 25% (being crushed to 325 orders) through airslide disintegrating mill, and the 400000 Buddhist nun's Mycosporin powder 25% of tiring, kaolin 50%, the three is 180kg altogether, and it is standby that three kinds of compositions fully mix back sealing preservation.
Take by weighing respectively that to contain the Osthole amount be 50% common cnidium fruit P.E 40kg, the 400000 Buddhist nun's Mycosporin bulk drug 32kg (by effective content) that tire.With mixed solvent 80kg Osthole is dissolved earlier, add Buddhist nun's Mycosporin powder again and stir into the muddy material, add blended emulsifier 80kg at last, stir standby.Medicine curtain material gross weight 232kg.
With 620 kilograms of input comminutors of cupric sulphate crystal, speed of agitator 60-80 rev/min.6 sprays medicine curtain material and seed coating medicines spray medicine curtain material .38.7kg at every turn repeatedly, and preceding at every turn spread for 5 times mixed seed coating medicine 25kg, and last dressing is with mixing seed coating medicine 55kg.Sharedly remove to mix seed coating medicine 180kg.
Present embodiment produces snake gram water dispersion granule 999.5kg.Contain Osthole 2.0% after testing in the product.Buddhist nun's Mycosporin 5.02%.
Embodiment 11
Core is selected for use: white granulated sugar crystal 6 65kg;
Blended emulsifier is: Tween 80 70%, and calcium dodecyl benzene sulfonate 30%, the two common 85kg fully mixes;
Mixed solvent is: ethyl acetate 30%, and carrene 30%, methyl alcohol 30%, dimethyl sulfoxide (DMSO) 10%, the three is 70L altogether;
Mixing seed coating medicine is: neopelex 20%, powdered glucose 30%, diatomite 50%, the three is 100kg altogether, mixing after airslide disintegrating mill to be crushed to 325 orders standby.
Production process is with reference to embodiment 10, and present embodiment usefulness contains the common cnidium fruit P.E 40kg of Osthole amount 50%, and the former medicine 50kg of Acetamiprid (by effective content) sprays medicine curtain and dressing 5 times repeatedly.49 kilograms of each spray medicine curtains spread 15 kilograms of seed coating medicines at every turn, use 40 kilograms of seed coating medicines for the last time for preceding 4 times.
Present embodiment produces snake pyridine water dispersion granule 1000kg, contains Osthole 2.0% in the product.Acetamiprid 5.0%.
Embodiment 12
Core is selected for use: urea 750kg;
Blended emulsifier is: polysorbate60 70%, and calcium dodecyl benzene sulfonate 30%, the two common 20kg fully mixes;
Mixed solvent is: acetone and carrene (1: 1 volume) are formed mixed solvent, the two common 60L.
Mixing seed coating medicine is: dodecyl sodium sulfate 20%, soluble starch 30%, white carbon black 50%.The three is 140kg altogether, the former two's raw material after airslide disintegrating mill is crushed to 325 orders with the white abundant mixing of carbon black after standby.
Production process is with reference to embodiment 3.The present embodiment common cnidium fruit P.E 41kg that contains Osthole amount 50%, 95% eliminates former medicine 22kg, forms medicine curtain material 142kg.With reference to embodiment 3 spraying medicine curtain and seed coating medicines.
Present embodiment produces snake and removes water dispersion granule 1030kg, after testing, contains Osthole 1.98%. in the product and contains and eliminate 2.02%.
Embodiment 13
Core is selected for use: urea granules 672kg;
Blended emulsifier is: polysorbate60 40%, and agricultural emulsifier NO 60%, the two common 64kg fully mixes;
Mixed solvent is: methyl alcohol 45%, and ethyl acetate 45%, acetone 10%, the three is 80L altogether;
Mixing seed coating medicine is: dodecyl sodium sulfate 20%, tpn soluble powder (70% content) 40%, white carbon black 40%, the three is 170kg altogether, dodecyl sodium sulfate is crushed to behind 325 orders fully to mix with the tpn of identical fineness and white carbon black three form.
Take by weighing tpn raw material 54kg (by effective content),, add the common cnidium fruit P.E 40kg that contains Osthole amount 50% again, stir with the mixed solvent dissolving.Add blended emulsifier at last, continue to stir, be medicine curtain material until becoming transparent slurry.
Method by embodiment 7 is carried out granulation.Spray medicine curtain material and dressing 5 times repeatedly spray medicine curtain material 47.6kg at every turn, spread seed coating medicine 30kg at every turn, spread seed coating medicine 50kg for the last time for preceding 4 times.
Present embodiment produces snake clear water dispersible granule 1001.2kg, contains Osthole 1.98% after testing in the product.Tpn 10.14%.
Embodiment 14
Core is selected for use: urea granules 744kg;
Blended emulsifier is: Tx-10 65%, farming breast No. 500 35%, and the two common 75kg fully mixes;
Mixed solvent is: absolute ethyl alcohol 70%, ethyl acetate 30%, the two common 60L;
Mixing seed coating medicine is: white carbon black 50%, and sericite in powder 30%, dodecyl sodium sulfate 20%, the three is 130kg altogether, and back two kinds of compositions are wanted fully to mix standby with white carbon black after airslide disintegrating mill is crushed to 325 orders earlier.
Take by weighing the common cnidium fruit P.E 50kg that contains Osthole amount 80%, the former medicine 1kg of compound sodium nitrophenolate (by effective content) adds and adds blended emulsifier again after mixed solvent fully dissolves it, fully stirs into uniform medicine curtain material, heavy altogether 186kg.
Method by embodiment 10 is carried out granulation.Repeat spray and dressing for five times, spray medicine curtain material 37.2kg at every turn, preceding 4 dressings are used seed coating medicine 28kg at every turn, last dressing seed coating medicine 38kg.
Present embodiment is produced the multiple glass gall dispersible granule 1000kg of snake.After testing, contain Osthole 4.0% in the product, contain compound sodium nitrophenolate 0.1%.
Experimental example 1
In two years, successively (field) application test of different objects has carried out in the field with the trial product of being produced among above-mentioned 14 embodiment.The emulsion of establishing identical effective ingredient in the test is medicament in contrast.Suitable substantially by the water dispersion granule effect of testing common cnidium fruit P.E as can be known with the contrast medicament.Data see Table 2.
Table 2 common cnidium fruit P.E water dispersion granule compares with contrast medicament field efficacy
| The embodiment sequence number | Controlling object | Spray effective component content in the soup | (%) imitated in the side of granule | Contrast pharmacy control efficacy (%) | Conclusion (of pressure testing) |
| Example 1 | Powdery mildew of strawberry | Osthole 10 (μ g/ml) generation high by 75 (μ g/ml) | 86.7 | 84.3 | No significant difference |
| Example 2 | Cabbage caterpillar | Osthole 42 (μ g/ml) B.t 32IU/ml | 95.5 | 95.1 | No significant difference |
| Example 3 | Alternaria alternate | Osthole 80 (μ g/ml) | 79.4 | 75.2 | No significant difference |
| Example 4 | Sclerotinia rot of colza | Osthole 60 (μ g/ml) | 82.7 | 77.6 | No significant difference |
| Example 5 | Vegetable aphid | Osthole 80 (μ g/ml) | 97.9 | 98.8 | No significant difference |
| Example 6 | Tea geometrid | Osthole 15 (μ g/ml) time 20 (μ g/ml) | 100 | 100 | No significant difference |
| Example 7 | Diamond-back moth | The sharp strength spy 20 of Osthole 20 (μ g/ml) (μ g/ml) | 90.1 | 88.5 | No significant difference |
| Example 8 | The eggplant two spotted spider mite | Osthole 10 (μ g/ml) Avermectin B 110(μg/ml) | 100 | 100 | No significant difference |
| Example 9 | Alternaria alternate | Osthole 20 (μ g/ml) Polyoxin 30 (μ g/ml) | 90.6 | 91.7 | No significant difference |
| Example 10 | Alternaria leaf spot of apple | Osthole 20 (μ g/ml) Buddhist nun's Mycosporin 50 (μ g/ml) | 84.5 | 81.9 | No significant difference |
| Example 11 | Wheat aphid | Osthole 20 (μ g/ml) Acetamiprid 50 (μ g/ml) | 96.7 | 97.2 | No significant difference |
| The embodiment sequence number | Controlling object | Spray effective component content in the soup | (%) imitated in the side of granule | Contrast pharmacy control efficacy (%) | Conclusion (of pressure testing) |
| Example 12 | Rice leaf roller | Osthole 30 (μ g/ml) eliminates 30 (μ g/ml) | 92.0 | 89.5 | No significant difference |
| Example 13 | Cucumber downy mildew | Osthole 20 (μ g/ml) tpn 100 (μ g/ml) | 87.3 | 86.8 | No significant difference |
| Example 14 | Graw mold of tomato | Osthole 40 (μ g/ml) compound sodium nitrophenolate 1 (μ g/ml) | 82.1 | 83.4 | No significant difference |
Experimental example 2
At the indoor antibacterial and insecticidal effect that has compared granule of the present invention and traditional emulsifiable concentrate, find that the effect and the missible oil of granule does not have remarkable difference, data see Table 3.
The indoor specific activity of table 3 frutus cnidii granule and emulsifiable concentrate
Experimental example 3
This granule and traditional missible oil are carried out field control effect relatively under the same concentrations condition, the result shows that the effect of Osthole granule is suitable with emulsifiable concentrate, or slightly is better than missible oil, and data see Table 4.
Table 4 Osthole granule and emulsifiable concentrate field control effect are relatively
Experimental example 4
Composite frutus cnidii granule and pure common cnidium fruit P.E emulsifiable concentrate are carried out field efficacy relatively under Osthole concentration the same terms, the result shows that various composite dose the effect of enumerating among the present invention all is better than the effect of pure common cnidium fruit P.E preparation, and data see Table 5.
Frutus cnidii granule that table 5 is composite and pure common cnidium fruit P.E missible oil field result of use are relatively
*: B.t. is the former powder of B.t.a, and metering is measured with international virulence unit.
Claims (4)
1. the water dispersion granule of a pesticide-germicide, it be by by weight or the following raw materials according of volume proportion prepare: in common cnidium fruit P.E 0.4-10 part of Osthole content, other pesticide-germicide materials 0-20 part, mixed solvent 2-20 part, blended emulsifier 1.5-15 part, mix seed coating medicine 4-15 part and core 40-90 part, described other pesticide-germicide materials are selected from pleocidin, intend the worm chrysanthemum ester insecticide, urea insecticide, organophosphorus insecticides, perhaps generation height, lucky star, tpn, phonetic mould amine, Polyoxin, in Buddhist nun's Mycosporin one or more; Described mixed solvent is selected from the 2-4 kind in methyl alcohol, ethanol, ethyl acetate, monochloro methane, carrene, dimethyl sulfoxide (DMSO) and the acetone; It is in 616 polyoxyethylene nonylphenol ether, polysorbate40, polysorbate60, Tween 80, anionic dodecyl sodium sulfate and the calcium dodecyl benzene sulfonate two kinds that described blended emulsifier is selected from mean molecule quantity; Described mixing seed coating medicine is the 3-4 kind that is selected from bacillus thuringiensis bacterium powder, compound sodium nitrophenolate, Acetamiprid, white carbon black, diatomite, kaolin, cellulose, soluble starch and the dodecyl sodium sulfate.
2. water dispersion granule as claimed in claim 1 is characterized in that described common cnidium fruit P.E obtains with carbonic acid gas critical point extraction.
3. water dispersion granule as claimed in claim 1 is characterized in that described core is selected from urea, boron fertilizer, KCl, sucrose, granule shape compound sodium nitrophenolate, NH
4H
2PO
4, C
uSO
4, fine granularity generation senior middle school one or more.
4. as the arbitrary described water dispersion granule of claim 1-3, it is characterized in that it prepares by following step:
(1) pulverizing that mixes seed coating medicine with mix: will be crushed to more than 325 orders behind the various composition mixings except that white carbon black, and/or carbon black mixes in vain;
(2) preparation of mixed solvent;
(3) dissolving of active substance with mix: dissolve common cnidium fruit P.E and other composite active substances respectively with mixed solvent, again with the two solution mixing;
(4) blended emulsifier and active substance mixed solution are fully mixed;
(5) under agitation step (4) gained compound is evenly sprayed to the core surface;
(6) under agitation will mix seed coating medicine and repeatedly be sprayed on step (5) the gained shot-like particle in batches, and continue after the been sprayed to stir 12-18 minute.
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| CN200610011311A CN101011051B (en) | 2006-02-05 | 2006-02-05 | Water dispersion granule for disinsection |
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| CN200610011311A CN101011051B (en) | 2006-02-05 | 2006-02-05 | Water dispersion granule for disinsection |
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| CN101011051B true CN101011051B (en) | 2010-05-12 |
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Families Citing this family (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100409747C (en) * | 2006-12-11 | 2008-08-13 | 江苏省农业科学院 | Application of osthole and its re-compound in preparing pesticide for preventing and controlling rice green smut |
| CN101878764A (en) * | 2010-06-23 | 2010-11-10 | 江苏省绿盾植保农药实验有限公司 | Compound insecticide containing pymetrozine and compound sodium nitrophenolate and preparation method thereof |
| CN102599150B (en) * | 2011-01-25 | 2013-09-04 | 郑州农达生化制品有限公司 | Plant growth regulator |
| CN102134174A (en) * | 2011-04-07 | 2011-07-27 | 枣庄市沃丰化工有限公司 | Organic insecticide envelope pesticide fertilizer and manufacturing technique |
| CN102383304B (en) * | 2011-06-22 | 2013-07-24 | 刘骁 | Household textile product with insecticidal effect and processing method thereof |
| CN103598214B (en) * | 2013-11-21 | 2015-02-25 | 薛刚 | Medicinal composition and method for preventing and controlling growth of moss in fritillaria planting greenhouse |
| CN104304255B (en) * | 2014-11-11 | 2016-06-08 | 南京科维邦农药有限公司 | A kind of antibacterial on Bulbus Allii |
| CN104351187B (en) * | 2014-11-11 | 2016-08-24 | 青岛青知企业管理咨询有限公司 | Active ingredient is the compound disinfectant of Osthole and pyrimethanil |
| CN104304256B (en) * | 2014-11-11 | 2016-08-17 | 青岛青知企业管理咨询有限公司 | A kind of compositions for preventing and treating gray mold |
| CN104351188B (en) * | 2014-11-11 | 2016-09-07 | 青岛青知企业管理咨询有限公司 | A kind of microcapsule suspending agent for preventing and treating gray mold |
| CN104548113B (en) * | 2014-12-11 | 2017-12-01 | 天津博科林药品包装技术有限公司 | A kind of production technology of film coating agent |
| CN105815340A (en) * | 2016-04-29 | 2016-08-03 | 山东胜伟园林科技有限公司 | Insecticide for preventing and treating wheat diseases and pests and preparation method of insecticide |
| CN106538556A (en) * | 2016-09-30 | 2017-03-29 | 赵青娇 | A kind of biological pesticide of preventing and treating root-knot nematode |
| CN107306989A (en) * | 2017-05-16 | 2017-11-03 | 广西南宁黑泥巴农业科技有限公司 | A kind of pesticide synergistic composition containing Osthole |
| CN110278970B (en) * | 2019-07-31 | 2020-12-22 | 黑龙江省农业科学院植物保护研究所 | Chinese herbal medicine type seed coating agent and preparation method thereof |
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| CN1342412A (en) * | 2001-10-25 | 2002-04-03 | 武汉绿世纪生物工程有限责任公司 | Application of cnidium fruit extract in preparing agricultural pesticide |
| CN1488254A (en) * | 2002-10-11 | 2004-04-14 | 华中农业大学 | Aju water dispersion granule and production method thereof |
| CN1669422A (en) * | 2005-03-14 | 2005-09-21 | 武汉绿世纪生物工程有限责任公司 | Methylamino avermectin benzoate water dispersant granule and preparation method thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1342412A (en) * | 2001-10-25 | 2002-04-03 | 武汉绿世纪生物工程有限责任公司 | Application of cnidium fruit extract in preparing agricultural pesticide |
| CN1488254A (en) * | 2002-10-11 | 2004-04-14 | 华中农业大学 | Aju water dispersion granule and production method thereof |
| CN1669422A (en) * | 2005-03-14 | 2005-09-21 | 武汉绿世纪生物工程有限责任公司 | Methylamino avermectin benzoate water dispersant granule and preparation method thereof |
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