CN101999346A - Emulsifiable granule containing etofenprox composition and preparation method thereof - Google Patents

Emulsifiable granule containing etofenprox composition and preparation method thereof Download PDF

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CN101999346A
CN101999346A CN 201010592522 CN201010592522A CN101999346A CN 101999346 A CN101999346 A CN 101999346A CN 201010592522 CN201010592522 CN 201010592522 CN 201010592522 A CN201010592522 A CN 201010592522A CN 101999346 A CN101999346 A CN 101999346A
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chrysanthemum ester
ether chrysanthemum
ester composition
emulsification granula
preparation
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CN101999346B (en
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姜欣
冀京民
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SHANXI LVHAI AGROCHEMICAL CO Ltd
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SHANXI LVHAI AGROCHEMICAL CO Ltd
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Abstract

The invention provides an emulsifiable granule containing an etofenprox composition and a preparation method thereof, and relates to an agricultural insecticide and a preparation method thereof. The emulsifiable granule comprises the following raw materials in weight percentage: 1%-15% of active constituents, 5%-30% of wetting dispersing agents, 0-10% of solvents, 5%-40% of adsorbents, 0-10% of binders and the balance of carriers. The preparation method comprises the following steps of: uniformly mixing the active constituents and the liquid assistant in the formula, and making the mixture adsorbed on the carriers, mixing the mixture with other solid constituents, pulverizing the mixture by using an airflow pulverizer so that the grain size of the mixture reaches 98%, sieving the mixture by using a sieve of 45 mum, and then kneading and pelleting. Alternatively, the method comprises the following steps of: uniformly mixing the active constituents, the solvents and the liquid assistant in the formula, making the mixture uniformly adsorbed on solid constituents and carriers pulverized to the grain size of 98% so as to pass through sieving holes of 45 mum, and then kneading and pelleting. The emulsifiable granule solves the problems of short effect taking time and environmental pollution of the traditional etofenprox and pymetrozine insecticide.

Description

But a kind of emulsification granula and preparation method who contains ether chrysanthemum ester composition
Technical field
The present invention relates to agricultural insecticide and preparation method thereof, but relate to a kind of emulsification granula that contains ether chrysanthemum ester composition and preparation method thereof particularly.
Background technology
Long-term actual agriculture experience shows, on the one hand, repeats and single-mindedly uses a kind of reactive compound and come pest control, can produce resistance to particular active compounds under many circumstances, and the preventive effect of medicament is reduced.Usually will have the compound combination of the different mechanisms of action, can prolong the service life of active component.On the other hand, the insecticide that present protective plant is used generally adopts missible oil, suspending agent and wetting powder, though missible oil good drug efficacy, it is relatively easy to prepare, easy to use, but contain organic solvents such as a large amount of toluene, dimethylbenzene in the missible oil, environmental pollution is serious, and all has hidden danger in processes such as production, storage, transportation; Wetting powder has a large amount of dust in producing, using, contaminated environment influences operating personnel's health; Suspending agent exists bin stability relatively poor, and drug effect is not as good as missible oil.
Ether chrysanthemum ester (etofenprox) though structure in do not have chrysanthemumic acid, but because of space structure and pyrethroid have similarity, so still be called pyrethroid insecticides, have that insecticidal spectrum is wide, insecticidal activity is high, knock down that speed is fast, the lasting period is long, to aquatic organism low toxicities such as fish, less to natural enemy lethality such as paddy field spiders, to advantages such as crop safeties.Insect there is not the interior conduction of inhaling, invalid to the acarid control.Main preparation is: formulations such as missible oil, finish, ultra-low-volume formulation, suspending agent, wetting powder.Its chemical name and structural formula are as follows: 2-(4-ethoxyl phenenyl)-2-methyl-propyl-3-benzyloxy phenoxy base ether.
Figure BSA00000388755200011
Pyrrole aphid ketone (pymetrozine) belongs to pyridines or Triazinone insecticide, is the brand-new non-insects agent of killing livestock, and insect is had action of contace poison, also has systemic activity simultaneously.Can also can be in plant corpus in the phloem transporting in the xylem transporting.Be mainly used in control most of homoptera pest, especially aphid section, Aleyrodidae, Cicadellidae and Delphacidae insect insect, be applicable to vegetables, paddy rice, cotton, fruit tree and multiple field crop.Main preparation is: formulations such as water dispersible granules, suspending agent, wetting powder.Its chemical name and structural formula are as follows: 4, and 5-dihydro-6-methyl-4-(3-pyridine methylene amino)-1,2,4-3 (2H)-ketone.
Figure BSA00000388755200021
The formulation of ether chrysanthemum ester that uses and pyrrole aphid ketone has certain negative effect recommending to exist insecticidal effect not good enough on the using dosage to environment at present.Therefore, be necessary to develop a kind of environmentally friendly, good disinsection effect, and to the desinsection formulation kind of crop safety height such as paddy rice, brassicaceous vegetable, use cost economy, to satisfy the needs of agricultural production.But the emulsification granula is exactly a kind of novel form that grows up on this basis, advantage with solid pharmaceutical preparation and liquid preparation, be the more comprehensive product of combination property in the current pesticidal preparations, the exploitation of this environmental protection novel form will further strengthen its safety to environment, people and animals, crop.But do not see the report of concrete emulsification granula that openly contains ether chrysanthemum ester composition and preparation method thereof so far.
Summary of the invention
But the purpose of this invention is to provide a kind of emulsification granula and preparation method who contains ether chrysanthemum ester composition, the invention solves the problem that the performance of existing ether chrysanthemum ester, pyrrole aphid ketone insecticidal preparation medicine drug effect is insufficient, the feature of environmental protection is relatively poor.
The objective of the invention is to: on the one hand, but the emulsification granula that contains ether chrysanthemum ester composition of a kind of safety, environmental protection, stable storage, good disinsection effect is provided, improves its quick-acting, lasting period extended period, reduce spraying times, to reach the purpose of the control efficiency that significantly improves crop pests.On the other hand, but a kind of preparation method who contains the emulsification granula of ether chrysanthemum ester Pesticidal combination is provided.
For realizing goal of the invention, the present invention adopts following technical scheme: but a kind of emulsification granula that contains ether chrysanthemum ester composition, form by following raw materials by weight percent: active ingredient 1~50%, wetting dispersing agent 5~30%, solvent 0~10%, adsorbent 5~40%, binding agent 0~10%, carrier surplus.
Described effective ingredient is ether chrysanthemum ester and pyrrole aphid ketone mixed thing, and the portion rate that the relative scale that ether chrysanthemum ester and pyrrole aphid ketone are mixed is based on active component weight is 2: 3.
But effective ingredient ether chrysanthemum ester and pyrrole aphid ketone mixed thing are 10%~30% of emulsification granula weight ratio.
Wetting dispersing agent is a kind of in the following material or at least two kinds: naphthalenesulfonic acid-formaldehyde condensate (dispersant NNO), sodium lignin sulfonate, calcium lignosulfonate, methyl naphthalene sulfonate formaldehyde condensate (Dispersant MF), the sodium salt of alkyl naphthalene sulfonic acid condensation polymer (dispersant D425), anion and the non-ionic surface active agent compound (agricultural newborn 0201B) of solvent, castor oil polyoxyethylene ether (agricultural newborn BY110), alkyl phenyl APEO (farming breast 100), dibutyl naphthalene sulfonic acids calcium (farming breast 2201), calcium dodecyl benzene sulfonate (farming breast 500), alkyl phenol formaldehyde resin polyoxyethylene ether (Nongru-700), phenethyl phenol polyethenoxy polyethenoxy ether (farming breast 1601), castor oil polyoxyethylene (40) ether (agricultural newborn EL-40).
Described solvent is a kind of of following material: N-Methyl pyrrolidone, solvent naphtha, dimethylbenzene, toluene, N, dinethylformamide.
Adsorbent is a kind of of following material or at least two kinds: white carbon, bentonite, diatomite, attapulgite.
Described carrier is a kind of of following material or at least two kinds: precipitated calcium carbonate, talcum, potter's clay, kaolin, atlapulgite.
Adhesive is a kind of of following natural or synthetic material: xanthans, polyethylene glycol, dextrin, gelatin, polyvinyl alcohol, soluble starch, phenolic resins, shellac, carboxymethyl cellulose, methylcellulose and sodium alginate.
But a kind of preparation method who contains the emulsification granula of ether chrysanthemum ester composition, raw material is made up of following raw materials by weight percent: active ingredient 1~50%, wetting dispersing agent 5~30%, solvent 0~10%, adsorbent 5~40%, binding agent 0~10%, carrier surplus; Method is: be adsorbed on the carrier earlier after active ingredient, liquid adjuvants component mix in will filling a prescription earlier, again with after other solid constituent is mixed, pulverize by airslide disintegrating mill, make it granularity and reach 98%, then through kneading, granulation by 45 μ m sieve apertures.
Further, but a kind of preparation method who contains the emulsification granula of ether chrysanthemum ester composition of the present invention, can also be: raw material be made up of following raw materials by weight percent: active ingredient 1~50%, wetting dispersing agent 5~30%, solvent 0~10%, adsorbent 5~40%, binding agent 0~10%, carrier surplus; Method is: in will filling a prescription earlier behind active ingredient, solvent and the liquid adjuvants mixing, evenly be adsorbed on then on the component that is crushed to the carrier of granularity 98% by 45 μ m sieve apertures and solid mixture, then through kneading, granulation.
But contain the emulsification granula of ether chrysanthemum ester Pesticidal combination by the present invention that above-mentioned two kinds of methods are prepared, the performance of its product is not influenced by the preparation method all.
But the ether chrysanthemum ester composition emulsification granula that contains of the present invention can directly be converted the spraying use of water dilution back before use by the user.
Technique effect of the present invention is: but the ether chrysanthemum ester composition emulsification granula that contains of the present invention, when dilute with water, active ingredient is disperseed well, can in water, form a kind of common oil-in-water (O/W) type emulsion, because the emulsion particle diameter that forms is very little, can be absorbed rapidly by plant, thereby make the drug effect of active ingredient be not fully exerted, reduce using dosage.
But of the present inventionly contain ether chrysanthemum ester composition emulsification granula compared with prior art, have the following advantages: 1) good fluidity, non-caked, do not lump.Be easy to packing and use, production, storage, transportation safety, environmentally friendly, to operator's safety; 2) but the preparation its soup wetability of emulsification granula good, the biologically active height, quick-acting is good, the lasting period is long, safety is good; 3) preparation method is simple, uses conveniently.
Embodiment
With illustrated embodiments the present invention is done detailed explanation below.
But the preparation method of the present invention's emulsification granula, can process preparation as the case may be, a kind of method is: after active ingredient, solvent, liquid adjuvants component mix in will filling a prescription earlier, join while stirring in advance in the container that carrier and other solid constituent are mixed, make it be adsorbed on the solid mixture equably, then, pulverize by airslide disintegrating mill, make it granularity and reach 98% by 45 μ m sieve apertures, last, add a certain amount of binding agent, through kneading, granulation; Another kind method is: in will filling a prescription earlier behind active ingredient, solvent and the liquid adjuvants mixing, evenly be adsorbed on then and be crushed in advance on granularity 98% carrier and the component of solid mixture by 45 μ m, then, add a certain amount of binding agent, through kneading, granulation.Product after the granulation behind fluid-bed drying, screening, detects packing, but contains the emulsification granula of ether chrysanthemum ester composition by the present invention that above-mentioned two kinds of methods are prepared, and the performance of its product is not influenced by the preparation method all.
Following instantiation is in order to detailed description the present invention, but the present invention only limits to these examples absolutely not.Percentage all is weight percentage in the proportioning of all preparations.
Embodiment 1
But 10% ether chrysanthemum ester pyrrole aphid ketone emulsification granula
Ether chrysanthemum ester 4%
Pyrrole aphid ketone 6%
Sodium lignin sulfonate 3%
Lauryl sodium sulfate 2%
Dispersant D425 3%
The newborn 0201B 3% of farming
White carbon 20%
Dimethylbenzene 6%
Diatomite complements to 100%
Embodiment 2
But 15% ether chrysanthemum ester pyrrole aphid ketone emulsification granula
Ether chrysanthemum ester 5%
Pyrrole aphid ketone 10%
Dimethylbenzene 10%
The newborn 0201B 6% of farming
Farming breast 2,201 3%
Neopelex 1%
Naphtholsulfonic acid formaldehyde condensation products 10%
Bentonite 10%
Carboxymethyl cellulose 1%
Atlapulgite complements to 100%
Embodiment 3
But 20% ether chrysanthemum ester pyrrole aphid ketone emulsification granula
Ether chrysanthemum ester 8%
Pyrrole aphid ketone 12%
Dimethylbenzene 10%
The newborn 0201B 8% of farming
Farming breast 1,601 2%
White carbon 20%
The sodium salt 5% of alkyl naphthalene sulfonic acid condensation polymer
Sodium lignin sulfonate 3%
PEG400 1%
Kaolin complements to 100%
Embodiment 4
But 30% ether chrysanthemum ester pyrrole aphid ketone emulsification granula
Ether chrysanthemum ester 12%
Pyrrole aphid ketone 18%
N-Methyl pyrrolidone 5%
The newborn 0201B 5% of farming
Nongru-700 2%
Farming breast 1,601 2%
White carbon 15%
Naphthalenesulfonic acid-formaldehyde condensate 6%
The sodium salt 5% of alkyl naphthalene sulfonic acid condensation polymer
Soluble starch 5%
Precipitated calcium carbonate complements to 100%
Embodiment 5.
But 25% ether chrysanthemum ester pyrrole aphid ketone emulsification granula
Ether chrysanthemum ester 10%
Pyrrole aphid ketone 15%
Naphthalenesulfonic acid-formaldehyde condensate 4%
Sodium lignin sulfonate 3%
Dimethylbenzene 8%
The newborn 0201B 6% of farming
The newborn BY110 3% of farming
White carbon 20%
Bentonite 10%
Carboxymethyl cellulose 0.5%
Kaolin complements to 100%
Embodiment 6 (test of pesticide effectiveness)
Indoor biological activity test measurement result (preventing and treating rice hoppers)
Figure BSA00000388755200081
By the test of pesticide effectiveness result of last table as can be seen, but the emulsification granula that contains ether chrysanthemum ester composition of the present invention is compared with prior art, and it is remarkable to have an insecticidal effect, the biologically active height, and the lasting period is long.But the ether chrysanthemum ester composition emulsification granula that contains provided by the invention, safety in production, use, storage, transportation not only, and advantage such as it is simple to have processing technology, uses conveniently, environmentally friendly are a kind of desirable insecticide varieties.
Above embodiment is more preferably embodiment a kind of of the present invention, the common variation that those skilled in the art carry out in the technical program scope and replace and should be included in protection scope of the present invention.

Claims (10)

1. but an emulsification granula that contains ether chrysanthemum ester composition is characterized in that, is made up of following raw materials by weight percent: active ingredient 1~50%, wetting dispersing agent 5~30%, solvent 0~10%, adsorbent 5~40%, binding agent 0~10%, carrier surplus.
2. but a kind of emulsification granula that contains ether chrysanthemum ester composition as claimed in claim 1 is characterized in that, described effective ingredient is ether chrysanthemum ester and pyrrole aphid ketone mixed thing, and the portion rate that the relative scale that ether chrysanthemum ester and pyrrole aphid ketone are mixed is based on active component weight is 2: 3.
3. but a kind of emulsification granula that contains ether chrysanthemum ester composition as claimed in claim 2 is characterized in that, but effective ingredient ether chrysanthemum ester and pyrrole aphid ketone mixed thing are 10%~30% of emulsification granula weight ratio.
4. but a kind of emulsification granula that contains ether chrysanthemum ester composition as claimed in claim 1, it is characterized in that wetting dispersing agent is a kind of in the following material or at least two kinds: naphthalenesulfonic acid-formaldehyde condensate, sodium lignin sulfonate, calcium lignosulfonate, methyl naphthalene sulfonate formaldehyde condensate, the sodium salt of alkyl naphthalene sulfonic acid condensation polymer, anion and the non-ionic surface active agent compound of solvent, castor oil polyoxyethylene ether, the alkyl phenyl APEO, dibutyl naphthalene sulfonic acids calcium, calcium dodecyl benzene sulfonate, alkyl phenol formaldehyde resin polyoxyethylene ether, phenethyl phenol polyethenoxy polyethenoxy ether, castor oil polyoxyethylene 40 ethers.
5. but a kind of emulsification granula that contains ether chrysanthemum ester composition as claimed in claim 1 is characterized in that described solvent is a kind of of following material: N-Methyl pyrrolidone, solvent naphtha, dimethylbenzene, toluene, N, dinethylformamide.
6. but a kind of emulsification granula that contains ether chrysanthemum ester composition as claimed in claim 1 is characterized in that, adsorbent is a kind of in the following material or at least two kinds: white carbon, bentonite, diatomite, attapulgite.
7. but a kind of emulsification granula that contains ether chrysanthemum ester composition as claimed in claim 1 is characterized in that, described carrier is a kind of of following material or at least two kinds: precipitated calcium carbonate, talcum, potter's clay, kaolin, atlapulgite.
8. but a kind of emulsification granula that contains ether chrysanthemum ester composition as claimed in claim 1, it is characterized in that adhesive is a kind of of following natural or synthetic material: xanthans, polyethylene glycol, dextrin, gelatin, polyvinyl alcohol, soluble starch, phenolic resins, shellac, carboxymethyl cellulose, methylcellulose and sodium alginate.
9. but a preparation method who contains the emulsification granula of ether chrysanthemum ester composition is characterized in that described raw material is made up of following raw materials by weight percent: active ingredient 1~50%, wetting dispersing agent 5~30%, solvent 0~10%, adsorbent 5~40%, binding agent 0~10%, the carrier surplus; Method is: be adsorbed on the carrier earlier after active ingredient, liquid adjuvants component mix in will filling a prescription earlier, again with after other solid constituent is mixed, pulverize by airslide disintegrating mill, make it granularity and reach 98%, then through kneading, granulation by 45 μ m sieve apertures.
10. but a preparation method who contains the emulsification granula of ether chrysanthemum ester composition is characterized in that described raw material is made up of following raw materials by weight percent: active ingredient 1~50%, wetting dispersing agent 5~30%, solvent 0~10%, adsorbent 5~40%, binding agent 0~10%, the carrier surplus; Method is: in will filling a prescription earlier behind active ingredient, solvent and the liquid adjuvants mixing, evenly be adsorbed on then on the component that is crushed to the carrier of granularity 98% by 45 μ m sieve apertures and solid mixture, then through kneading, granulation.
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Cited By (9)

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Publication number Priority date Publication date Assignee Title
CN102308794A (en) * 2011-05-18 2012-01-11 江西正邦生物化工股份有限公司 Carbosulfan emulsifiable granules and preparation method thereof
CN102308791A (en) * 2011-05-18 2012-01-11 江西正邦生物化工股份有限公司 Prochloraz emulsifiable granules and preparation method thereof
CN102308796A (en) * 2011-05-18 2012-01-11 江西正邦生物化工股份有限公司 Diazinon emulsifiable granules and preparation method thereof
CN102308792A (en) * 2011-05-18 2012-01-11 江西正邦生物化工股份有限公司 Propiconazole emulsifiable granules and preparation method thereof
CN102308795A (en) * 2011-05-18 2012-01-11 江西正邦生物化工股份有限公司 Profenofos emulsifiable granules and preparation method thereof
CN102308793A (en) * 2011-05-18 2012-01-11 江西正邦生物化工股份有限公司 Chlopyrifos emulsifiable granules and preparation method thereof
CN102919231A (en) * 2012-11-06 2013-02-13 山西绿海农药科技有限公司 Emulsible granule containing spirodiclofen composition and preparation method thereof
CN106070239A (en) * 2016-06-12 2016-11-09 创新美兰(合肥)股份有限公司 A kind of pymetrozine and ethofenprox compound suspending agent and preparation method thereof
CN107047548A (en) * 2017-03-28 2017-08-18 黑龙江华夏统联农业技术开发有限公司 A kind of anti-drift agent and the spray adjuvantses including it and its preparation method and application

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CN101731227A (en) * 2010-01-26 2010-06-16 江苏省绿盾植保农药实验有限公司 Compound pesticide containing etofenprox and pymetrozine

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Publication number Priority date Publication date Assignee Title
CN102308794A (en) * 2011-05-18 2012-01-11 江西正邦生物化工股份有限公司 Carbosulfan emulsifiable granules and preparation method thereof
CN102308791A (en) * 2011-05-18 2012-01-11 江西正邦生物化工股份有限公司 Prochloraz emulsifiable granules and preparation method thereof
CN102308796A (en) * 2011-05-18 2012-01-11 江西正邦生物化工股份有限公司 Diazinon emulsifiable granules and preparation method thereof
CN102308792A (en) * 2011-05-18 2012-01-11 江西正邦生物化工股份有限公司 Propiconazole emulsifiable granules and preparation method thereof
CN102308795A (en) * 2011-05-18 2012-01-11 江西正邦生物化工股份有限公司 Profenofos emulsifiable granules and preparation method thereof
CN102308793A (en) * 2011-05-18 2012-01-11 江西正邦生物化工股份有限公司 Chlopyrifos emulsifiable granules and preparation method thereof
CN102308791B (en) * 2011-05-18 2014-03-19 江西正邦生物化工股份有限公司 Prochloraz emulsifiable granules and preparation method thereof
CN102919231A (en) * 2012-11-06 2013-02-13 山西绿海农药科技有限公司 Emulsible granule containing spirodiclofen composition and preparation method thereof
CN102919231B (en) * 2012-11-06 2015-06-10 山西绿海农药科技有限公司 Emulsible granule containing spirodiclofen composition and preparation method thereof
CN106070239A (en) * 2016-06-12 2016-11-09 创新美兰(合肥)股份有限公司 A kind of pymetrozine and ethofenprox compound suspending agent and preparation method thereof
CN107047548A (en) * 2017-03-28 2017-08-18 黑龙江华夏统联农业技术开发有限公司 A kind of anti-drift agent and the spray adjuvantses including it and its preparation method and application
CN107047548B (en) * 2017-03-28 2020-11-13 黑龙江华夏统联农业技术开发有限公司 Anti-drift agent, spraying aid comprising anti-drift agent, and preparation method and application of spraying aid

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