CN101578039B - Insecticidal water soluble granule of fipronil and preparation thereof - Google Patents
Insecticidal water soluble granule of fipronil and preparation thereof Download PDFInfo
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- CN101578039B CN101578039B CN 200880000077 CN200880000077A CN101578039B CN 101578039 B CN101578039 B CN 101578039B CN 200880000077 CN200880000077 CN 200880000077 CN 200880000077 A CN200880000077 A CN 200880000077A CN 101578039 B CN101578039 B CN 101578039B
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- worm nitrile
- fluorine worm
- disinsection
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- soluble granula
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N47/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid
- A01N47/02—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid the carbon atom having no bond to a nitrogen atom
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- Life Sciences & Earth Sciences (AREA)
- Agronomy & Crop Science (AREA)
- Pest Control & Pesticides (AREA)
- Plant Pathology (AREA)
- Health & Medical Sciences (AREA)
- Engineering & Computer Science (AREA)
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- General Health & Medical Sciences (AREA)
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Abstract
The invention provides a water soluble granule of fipronil, which is made from (by wt%) fipronil 0.5-50%, emulsifier 1-30%, dispersing agent 1-10%, wetting agent 1-5%, binder 2-4%, stabilizer 1-3% andthe rest is filling material. The invention also provides the preparation method of the soluble granule of fipronil, which comprises kneading, extruding, granulating, vacuum drying at 70 DEG C for 1hour, screening and packaging. The product of the invention has a high insecticidal effect, is of low cost, is safe and convenient to use and is friendly to environment.
Description
Technical field
The present invention relates to a kind of disinsection soluble granula that contains fluorine worm nitrile and preparation method thereof, pesticide for protecting plant of particularly a kind of disinsection soluble granula that contains fluorine worm nitrile and preparation method thereof.
Background technology
Improving constantly of Along with people's living standard; People are to the raising of environmental protection consciousness; And the Chinese government is to the attention of ecotope, on the domestic and international market to be fit to controlling crop diseases and insect pests and nuisanceless production needs efficiently, the demand of low toxicity, low-residual, free of contamination environment protection biological agricultural chemicals and chemical pesticide is increasing.
The kind of pesticide for protecting plant is a lot, generally adopts missible oil and wetting powder.As everyone knows, contain a large amount of organic solvents in the missible oil, be easy to volatilization, catch fire, toxic to human body and plant, contaminated environment, transportation is also inconvenient; Wetting powder can produce a large amount of dust in producing, using, contaminated environment influences operating personnel's health.
Pesticidal preparations develops to solvent free, water baseization, solidification and multifunction direction, and disinsection soluble granula of the present invention just is being based on this developing direction development.
Summary of the invention
The object of the invention is exactly in order to overcome the shortcoming that above-mentioned prior art exists, a kind of safe in utilization, environmental protection to be provided, and the disinsection soluble granula is used in the plant protection that contains fluorine worm nitrile.
For solving the problems of the technologies described above, the present invention realizes through following technical scheme:
A kind of disinsection soluble granula that contains fluorine worm nitrile; Form by fluorine worm nitrile, emulsifier, dispersant, wetting agent, binding agent, stabilizing agent and filler; In soluble granula weight is 100%, and it is formed content and is: fluorine worm nitrile 0.5～50%, emulsifier 1～30%, dispersant 1～10%, wetting agent 1～5%, binding agent 2～4%, stabilizing agent 1～3%, all the other are fillers.
Described emulsifier is selected from APES, like NPE and OPEO etc.; Benzylphenol APEO and analog are like benzylphenol APEO and benzyl APES; AEO and analog are like C
nH
2n+1O (EO)
mH, wherein, n=12～16, m=15～30, it is to be the product of principal component with the laruyl alcohol; Span and ethylene oxide adduct thereof, like Span-20,40,60,65,80,85, Tween20,21,40,60,61,65,80,81 and 85 etc.
Described dispersant is selected from alkylnaphthalene sulfonate, as Nekal BX with draw back powder AC etc.; Two naphthalenesulfonate formaldehyde condensation compounds are like dispersant N and dispersant NNO etc.; And sodium lignin sulfonate.
Described wetting agent is selected from one or both in alkylbenzenesulfonate, fatty acid amide N-metilsulfate and the alkylaryl polyoxyethylene ether sulfate.
Described binding agent is selected from one or both in beta-schardinger dextrin-, polyvinyl alcohol, methylcellulose, glucose and the urea.
Described stabilizing agent is selected from a kind of in Sodium Benzoate and the glucose.
Described filler is selected from one or both in sodium bicarbonate, anhydrous citric acid, maltose and the anhydrous sodium sulfate.
A kind ofly prepare the above-mentioned method that contains the disinsection soluble granula of fluorine worm nitrile, may further comprise the steps:
1. homogeneous: the former medicine of fluorine worm nitrile and binding agent, wetting agent are mixed in 50～60 ℃ of water, in 420～450 kilograms per centimeter
2High pressure stirs homogeneous down;
2. the aforesaid liquid mixture behind the homogeneous is carried out atomized drying, process compound female medicine;
3. mediate: after the emulsifier heat of solution, mix with dispersant, stabilizing agent, filler and compound female medicine heat under 45～50 ℃ of temperature, again in 4～6 kilograms per centimeter
2Pressure stirs down, mediates evenly, the group's of obtaining agent;
4. extruder grain: will roll into a ball agent in 6～12 kilograms per centimeter
2Extrude into cylindrical particle under the pressure;
5. cylindrical particle is sieved shaping 70 ℃ of following vacuum dryings after 1 hour.
Fluorine worm nitrile is a kind of Phenylpyrazole insecticides, and insecticidal spectrum is wide, is main to insect with stomach poison function, has concurrently and tags and certain systemic function, and its insecticidal mechanism is to hinder the chloride metabolism of insect GABA control.Therefore, important pests such as aphid, leafhopper, plant hopper, lepidopterous larvae, fly class and coleoptera there is very high insecticidal activity, crop is not had poisoning.This medicament can impose on soil, but also foliar spray.Impose on soil chrysomelid, wireworm of control of maize root and cutworm effectively.During foliage spray, diamond-back moth, imported cabbageworm and rice thrips etc. are all had high-level preventive effect, and the lasting period is long.
Insecticide of the present invention is compared with existing main flow insecticide formulation, does not contain or only contain poisonous, inflammable on a small quantity aromatic hydrocarbon solvent, thus can avoid producing with transporting procedures in inflammable and explosive phenomenon.This formulation does not have unpleasant poisonous smell, and is little to eye irritation, reduced the pollution to environment, improved the safety to production, storing and user greatly.Therefore, after the formation industrialization, not only economic benefit is obvious, and helps promoting the development of high-new environment friendly agricultural technology, to promoting environmental protection, has obvious social, is the Research on Sustainable Development direction.
Soluble granula is a kind of novel form, is the more comprehensive product of combination property in the current pesticidal preparations.Soluble granula is developed in success will further strengthen its safety to environment, people and animals, crop.Therefore various raw material sources all are common in the domestic Chemical market in the prescription, and product cost is lower, for the suitability for industrialized production of this formulation and apply and lay a good foundation.
Embodiment
Below in conjunction with specific embodiment the present invention is described further.
Embodiment 1
Prepare the disinsection soluble granula that contains fluorine worm nitrile of the present invention by following method:
1. 0.5% the former medicine of fluorine worm nitrile and 1% polyvinyl alcohol, 4% neopelex are mixed in 55 ℃ of water, in 420 kilograms per centimeter
2High pressure stirs homogeneous down;
2. the aforesaid liquid mixture behind the homogeneous is carried out atomized drying, process compound female medicine;
3. with after 3% the NPE heat of solution, mix with 3% dispersant NNO, 1% Sodium Benzoate, 46% sodium bicarbonate, 41.5% anhydrous citric acid and compound female medicine heat under 45 ℃ of temperature, again in 4 kilograms per centimeter
2Pressure stirs down, mediates evenly, the group's of obtaining agent;
4. will roll into a ball agent in 6 kilograms per centimeter
2Extrude into cylindrical particle under the pressure;
5. cylindrical particle is sieved after 1 hour 70 ℃ of following vacuum dryings, the product that sieves is packed after detecting; The product of not crossing sieve repeats above process again after detect qualified packing.
Be made into preparation according to the above ratio, every mu is used 300g, and good to the preventive effect of rice grub striped rice borer, paddy stem borer, rice leaf roller, control efficiency is as shown in the table.
Embodiment 2
Prepare the disinsection soluble granula that contains fluorine worm nitrile of the present invention by following method:
1. 10% the former medicine of fluorine worm nitrile and 1.2% beta-schardinger dextrin-, 4% fatty acid amide N-metilsulfate are mixed in 50 ℃ of water, in 430 kilograms per centimeter
2High pressure stirs homogeneous down;
2. the aforesaid liquid mixture behind the homogeneous is carried out atomized drying, process compound female medicine;
3. with after 6% xenol APEO, the 2% benzylphenol APEO heat of solution; Mix with 0.8% sodium lignin sulfonate, 1% borax, 42% sodium bicarbonate, 33% anhydrous sodium sulfate and compound female medicine heat under 45 ℃ of temperature, again in 5 kilograms per centimeter
2Pressure stirs down, mediates evenly, the group's of obtaining agent;
4. will roll into a ball agent in 8 kilograms per centimeter
2Extrude into cylindrical particle under the pressure;
5. cylindrical particle is sieved after 1 hour 70 ℃ of following vacuum dryings, the product that sieves is packed after detecting; The product of not crossing sieve repeats above process again after detect qualified packing.
Be made into preparation according to the above ratio, every mu is used 14g good to the preventive effect of rice grub striped rice borer, paddy stem borer, rice leaf roller, and control efficiency is as shown in the table.
Embodiment 3
Prepare the disinsection soluble granula that contains fluorine worm nitrile of the present invention by following method:
1. 30% the former medicine of fluorine worm nitrile and 1% methylcellulose, 4% dodecyl sodium naphthalene sulfonate are mixed in 60 ℃ of water, in 440 kilograms per centimeter
2High pressure stirs homogeneous down;
2. the aforesaid liquid mixture behind the homogeneous is carried out atomized drying, process compound female medicine;
3. with behind 9% benzyl APES, 2% the Span and ethylene oxide adduct heat of solution thereof; Mix with 3% Nekal BX, 1% borax, 20% maltose, 30% anhydrous citric acid and compound female medicine heat under 50 ℃ of temperature, again in 6 kilograms per centimeter
2Pressure stirs down, mediates evenly, the group's of obtaining agent;
4. will roll into a ball agent in 10 kilograms per centimeter
2Extrude into cylindrical particle under the pressure;
5. cylindrical particle is sieved after 1 hour 70 ℃ of following vacuum dryings, the product that sieves is packed after detecting; The product of not crossing sieve repeats above process again after detect qualified packing.
Be made into preparation according to the above ratio, every mu is used 5g good to the preventive effect of rice grub striped rice borer, paddy stem borer, rice leaf roller, and control efficiency is as shown in the table.
Embodiment 4
Prepare the disinsection soluble granula that contains fluorine worm nitrile of the present invention by following method:
1. 50% the former medicine of fluorine worm nitrile and 2% beta-schardinger dextrin-, 4% alkylaryl polyoxyethylene ether sulfate are mixed in 55 ℃ of water, in 450 kilograms per centimeter
2High pressure stirs homogeneous down;
2. the aforesaid liquid mixture behind the homogeneous is carried out atomized drying, process compound female medicine;
3. with after 9% AEO, 4% the OPEO heat of solution; Mix with 1% draw back powder AC, 2% dispersant N, 1% borax, 15% maltose, 12% anhydrous citric acid and compound female medicine heat under 45 ℃ of temperature, again in 6 kilograms per centimeter
2Pressure stirs down, mediates evenly, the group's of obtaining agent;
4. will roll into a ball agent in 12 kilograms per centimeter
2Extrude into cylindrical particle under the pressure;
5. cylindrical particle is sieved after 1 hour 70 ℃ of following vacuum dryings, the product that sieves is packed after detecting; The product of not crossing sieve repeats above process again after detect qualified packing.
Be made into preparation according to the above ratio, every mu is used 3.2g good to the preventive effect of rice grub striped rice borer, paddy stem borer, rice leaf roller, and control efficiency is as shown in the table.
Industrial applicibility
Fluorine worm nitrile water-soluble granule of the present invention has very high insecticidal activity to important pests such as aphid, leafhopper, plant hopper, lepidopterous larvae, fly class and coleopteras, and crop is not had poisoning.This medicament can impose on soil, but also foliar spray.Impose on soil chrysomelid, wireworm of control of maize root and cutworm effectively.During foliage spray, diamond-back moth, imported cabbageworm and rice thrips etc. are all had high-level preventive effect, and the lasting period is long.
Although combined preferred implementation that the utility model is illustrated already, it will be apparent to those skilled in the art that can be to selection and the proportioning change and the improvement of similar compound.But, compare with the present invention, if its its effect with of the present invention same or similar, such improvement all still belongs to protection scope of the present invention.
Claims (8)
1. disinsection soluble granula that contains fluorine worm nitrile; It is characterized in that forming by fluorine worm nitrile, emulsifier, dispersant, wetting agent, binding agent, stabilizing agent and filler; Said emulsifier is selected from APES; Benzylphenol APEO and analog, AEO and analog and Span and ethylene oxide adduct thereof; Said dispersant is selected from alkylnaphthalene sulfonate, two naphthalenesulfonate formaldehyde condensation compounds, and sodium lignin sulfonate; Said wetting agent is selected from one or both in alkylbenzenesulfonate, fatty acid amide N-metilsulfate and the alkylaryl polyoxyethylene ether sulfate; Said binding agent is selected from one or both in beta-schardinger dextrin-, polyvinyl alcohol, methylcellulose, glucose and the urea; Said stabilizing agent is selected from a kind of in Sodium Benzoate and the glucose; Said filler is selected from one or both in sodium bicarbonate, anhydrous citric acid, maltose and the anhydrous sodium sulfate; In soluble granula weight is 100%, and it is formed content and is: fluorine worm nitrile 0.5～50%, emulsifier 1～30%, dispersant 1～10%, wetting agent 1～5%, binding agent 2～4%, stabilizing agent 1～3%, all the other are fillers.
2. the disinsection soluble granula that contains fluorine worm nitrile according to claim 1 is characterized in that said APES is selected from NPE and OPEO.
3. the disinsection soluble granula that contains fluorine worm nitrile according to claim 1 is characterized in that said benzylphenol APEO and analog are selected from benzylphenol APEO and benzyl APES.
4. the disinsection soluble granula that contains fluorine worm nitrile according to claim 1 is characterized in that said AEO and analog are selected from C
nH
2n+1O (EO)
mH, wherein, n=12～16, m=15～30.
5. the disinsection soluble granula that contains fluorine worm nitrile according to claim 1; It is characterized in that said Span and ethylene oxide adduct thereof are selected from Span-20,40,60,65,80,85, Tween20,21,40,60,61,65,80,81 and 85.
6. the disinsection soluble granula that contains fluorine worm nitrile according to claim 1 is characterized in that said alkylnaphthalene sulfonate is selected from Nekal BX and draws back powder AC.
7. the disinsection soluble granula that contains fluorine worm nitrile according to claim 1 is characterized in that said pair of naphthalenesulfonate formaldehyde condensation compound is selected from dispersant N and dispersant NNO.
8. one kind prepares any said method that contains the disinsection soluble granula of fluorine worm nitrile among the claim 1-7, may further comprise the steps:
1. homogeneous: the former medicine of fluorine worm nitrile and binding agent, wetting agent are mixed in 50～60 ℃ of water, in 420～450 kilograms per centimeter
2High pressure stirs homogeneous down;
2. the aforesaid liquid mixture behind the homogeneous is carried out atomized drying, process compound female medicine;
3. mediate: after the emulsifier heat of solution, mix with dispersant, stabilizing agent, filler and compound female medicine heat under 45～50 ℃ of temperature, again in 4～6 kilograms per centimeter
2Pressure stirs down, mediates evenly, the group's of obtaining agent;
4. extruder grain: will roll into a ball agent in 6～12 kilograms per centimeter
2Extrude into cylindrical particle under the pressure;
5. cylindrical particle is sieved shaping 70 ℃ of following vacuum dryings after 1 hour.
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| PCT/CN2008/070113 WO2009089688A1 (en) | 2008-01-15 | 2008-01-15 | Water soluble granule of fipronil and its preparation |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101578039A CN101578039A (en) | 2009-11-11 |
| CN101578039B true CN101578039B (en) | 2012-12-05 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200880000077 Active CN101578039B (en) | 2008-01-15 | 2008-01-15 | Insecticidal water soluble granule of fipronil and preparation thereof |
Country Status (2)
| Country | Link |
|---|---|
| CN (1) | CN101578039B (en) |
| WO (1) | WO2009089688A1 (en) |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102308794B (en) * | 2011-05-18 | 2014-01-29 | 江西正邦生物化工股份有限公司 | Carbosulfan emulsifiable granules and preparation method thereof |
| GB2511318B (en) * | 2013-02-27 | 2015-12-30 | Rotam Agrochem Int Co Ltd | Agrochemical composition comprising pesticidally active pyrazole derivative with polyether adhesion promoter |
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| JP2004168784A (en) * | 1991-04-26 | 2004-06-17 | Nissan Chem Ind Ltd | Method for applying solid agrochemical preparation for flooded paddy field |
| GB0128722D0 (en) * | 2001-11-30 | 2002-01-23 | Syngenta Participations Ag | Seed treatment compositions |
| CN100518508C (en) * | 2005-05-18 | 2009-07-29 | 安徽华星化工股份有限公司 | Compound sterilization composition based on kresoxim methyl |
| CN1736197A (en) * | 2005-06-03 | 2006-02-22 | 栾贵书 | Water soluble granule of emamection benaoate and preparation method thereof |
| CN1775027A (en) * | 2005-11-21 | 2006-05-24 | 河北威远生物化工股份有限公司 | Disinsection soluble granules containing methylamino avermection benzoate |
| CN1957698A (en) * | 2006-11-24 | 2007-05-09 | 华南理工大学 | Water dispersion granules agent of Kresoxim and preparation method |
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2008
- 2008-01-15 WO PCT/CN2008/070113 patent/WO2009089688A1/en active Application Filing
- 2008-01-15 CN CN 200880000077 patent/CN101578039B/en active Active
Non-Patent Citations (3)
| Title |
|---|
| 慕卫等.抗高效氯氟氰菊酯甜菜夜蛾近等基因系的交互抗性和种群适合度.《中国农业科学》.2005,(第10期), * |
| 操海群等.氟虫腈在番茄和土壤中残留分析方法的研究.《安徽农业大学学报》.2005,(第01期), * |
| 许培骞等.防治稻纵卷叶螟高龄幼虫田间药效试验.《植物医生》.2005,(第05期), * |
Also Published As
| Publication number | Publication date |
|---|---|
| WO2009089688A1 (en) | 2009-07-23 |
| CN101578039A (en) | 2009-11-11 |
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