CN103238617A - Clothianidin synergia solubility granula and preparation method thereof - Google Patents
Clothianidin synergia solubility granula and preparation method thereof Download PDFInfo
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- CN103238617A CN103238617A CN2012102295003A CN201210229500A CN103238617A CN 103238617 A CN103238617 A CN 103238617A CN 2012102295003 A CN2012102295003 A CN 2012102295003A CN 201210229500 A CN201210229500 A CN 201210229500A CN 103238617 A CN103238617 A CN 103238617A
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- thiophene worm
- worm amine
- clothianidin
- soluble granule
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Abstract
The invention relates to a clothianidin synergia solubility granula and a preparation method thereof. The granula is prepared from the following components by weight percent: 1-20 percent of clothianidin, 1-10 percent of a dispersing agent, 1-5 percent of a wetting agent, 2-4 percent of a binder, 1-3 percent of a stabilizer, 1-3 percent of a synergist and the balance of fillings. The preparation method comprises the following steps of: carrying out coarse grinding on the clothianidin, dispersing agent, wetting agent, stabilizer and fillings, stirring and mixing, then carrying out ultrafine grinding to obtain ultrafine powder with the grain size less than 15 micrometers; and adding a binder for pelleting, screening by using a vibrating screen, and drying to obtain a product. The clothianidin synergia solubility granula has the advantages of the solid preparation and liquid pharmaceutical preparations; at the same time, due to the addition of synergist, the clothianidin synergia solubility granula has obviously control efficiency on the common crop injurious insects such as Hemiptera, coleopteran, diptera and certain lepidoptera pests, has the insecticidal efficacy improved by 1.4-1.5 times compared with that of the 50% clothianidin aqueous dispersion granula, and improves the utilization rate of the active constituent clothianidin.
Description
Technical field
The invention belongs to technical field of pesticide, relate to a kind of thiophene worm amine synergy soluble granule and preparation method thereof.
Background technology
Thiophene worm amine (English Clothianidin) belongs to anabasine insecticide, be a kind of active high, have interior absorption, tag and the broad spectrum pesticide of stomach poison function.For Semiptera, coleoptera, diptera and some Lepidoptera class pests such as the aphid on control paddy rice, vegetables, fruit tree and other crop, leafhopper, thrips, plant hoppers, have efficient, wide spectrum, consumption is few, toxicity is low (the little poison level of preparation), the lasting period is long, crop is not had poisoning, uses safety, do not have advantages such as cross resistance with conventional pesticide, is the another new varieties that substitute high malicious organophosphorous pesticide.
The thiophene worm amine insecticide that protective plant is used registration at present 50% thiophene worm amine water dispersible granules arranged.Because disintegration dissolving rapidly only can disperse to form particulate suspension after the water dispersible granules entry, utilization rate of active components is low, and generally speaking, the availability of active ingredient is about 70%.Result of study shows that disintegration fast solves homogeneously in and forms true solution in the water after the entry of synergy soluble granula, and solvability reaches more than 99%, and utilization rate of active components is more than 95%.In use soup can evenly be attached to plant leaf surface, and drug effect is apparently higher than water dispersible granules, is state-of-the-art formulation in the world at present, meets the developing direction of the international formulations of pesticide.
Summary of the invention
The purpose of this invention is to provide a kind of thiophene worm amine synergy soluble granule, improve the water-soluble energy of medicament, improve the drug effect of thiophene worm amine and the availability of active ingredient, another object of the present invention provides the preparation method of thiophene worm amine synergy soluble granule.
Thiophene worm amine synergy soluble granule of the present invention, be made up of following component by weight percentage: thiophene worm amine 1～20, dispersant 1～10, wetting agent 1～5, binding agent 2～4, stabilizing agent 1～3, synergist 1～3, surplus are filler.
Dispersant is sodium lignin sulfonate, sodium methylene bis-naphthalene sulfonate, fatty alcohol-polyoxyethylene ether or aliphatic alcohol sodium sulfate.Wetting agent is to methoxyl group fatty acyl amido benzene sulfonic acid sodium salt, lauryl sodium sulfate or sodium butylnaphthalenesulfonate.Binding agent is dextrin, polyethylene glycol or gelatin.Stabilizing agent is tbp or sodium hydrogen phosphate.Synergist is Escin, capsaicine, Butacide or triphenyl phosphate.Filler is maltose, glucose, soluble starch, Lactis Anhydrous or anhydrous sodium sulfate.
The preparation method of thiophene worm amine synergy soluble granule of the present invention, process is:
⑴ carry out coarse crushing with thiophene worm amine, dispersant, wetting agent, stabilizing agent, synergist and filler;
With coarse crushing after each component mix, carry out ultra-fine air-flow and pulverize, obtain the superfines of particle diameter below 15 microns;
⑶ add binding agent and carry out granulation;
⑷ sieve with vibratory sieve;
⑸ oven dry makes the granule product.
Bake out temperature is 60 ± 5 ℃, and drying time is 1～2 hour.
Thiophene worm amine synergy soluble granule of the present invention has the advantage of solid pharmaceutical preparation and liquid preparation concurrently, to common crop pests as Semiptera, coleoptera, diptera and some lepidoptera pest are had control efficiency significantly, the synergy soluble granule is compared insecticidal effect and is improved 1.4-1.5 times with 50% thiophene worm amine water dispersible granules, improved the availability of active principle thiophene worm amine.Thiophene worm amine synergy soluble granule low toxicity, harmless to people and animals, environment, crop, have safety in utilization.Auxiliary agent wide material sources of the present invention, the preparation method is simple, and production cost is low, is suitable for suitability for industrialized production and applies.
Embodiment
The present invention is described further below in conjunction with embodiment.
EXAMPLE l
The thiophene worm amine of weight portion 1%, 3% sodium lignin sulfonate dispersant, 2% the sodium hydrogen phosphate stabilizing agent to methoxyl group fatty acyl amido benzene sulfonic acid sodium salt wetting agent, l%, 2% capsaicine synergist and 89% maltose filler are pulverized the back mixing, and pulverize through air-flow, the dextrin binding agent of adding 2% is mediated and extruder grain, vacuum drying was sieved after 1 hour under 60 ℃ of temperature, and the product that sieves qualified back is after testing packed.Underproof product through pulverizing, is mediated and extruder grain again, screening after under 60 ℃ of temperature vacuum drying l hour, and the product that sieves qualified back packing is after testing made sample 1.
Embodiment 2.
The thiophene worm amine of weight portion 8%, 5% fatty alcohol-polyoxyethylene ether dispersant, 2% the glucose filler to methoxyl group fatty acyl amido benzene sulfonic acid sodium salt wetting agent, 1% tributyl phosphate stabilizing agent, 2% capsaicine synergist and 80% are pulverized the back to be mixed and pulverizes through air-flow, the dextrin binding agent of adding 2% is mediated and extruder grain, vacuum drying was sieved after 1 hour under 60 ℃ of temperature, and the product that sieves qualified back is after testing packed.Underproof product through pulverizing, is mediated and extruder grain again, screening after under 60 ℃ of temperature vacuum drying l hour, and the product that sieves qualified back packing is after testing made sample 2.
Embodiment 3
The soluble starch filler that the thiophene worm amine of weight portion 16%, 7% sodium lignin sulfonate dispersant, 3% lauryl sodium sulfate wetting agent, 1% tributyl phosphate are stablized chaste tree, 2% capsaicine synergist and 71% is pulverized the back and is mixed, and pulverize through air-flow, the polyethylene glycol binding agent of adding 2% is mediated and extruder grain, vacuum drying was sieved after 1 hour under 60 ℃ of temperature, and the product that sieves qualified back is after testing packed.Underproof product through pulverizing, is mediated and extruder grain again, screening after under 60 ℃ of temperature vacuum drying l hour, and the product that sieves qualified back packing is after testing made sample 3.
Embodiment 4
Thiophene worm amine with 20%, 8% sodium lignin sulfonate dispersant, 2% sodium butylnaphthalenesulfonate wetting agent, 1% sodium hydrogen phosphate stabilizing agent, 2% capsaicine synergist and 65% Lactis Anhydrous filler are pulverized the back and are mixed, and pulverize through air-flow, the gelatin binding agent of adding 2% is mediated and extruder grain, vacuum drying was sieved after 1 hour under 60 ℃ of temperature, and the product that sieves qualified back is after testing packed.Underproof product through pulverizing, is mediated and extruder grain again, screening after under 60 ℃ of temperature vacuum drying l hour, and the product that sieves qualified back packing is after testing made sample 4.
Performance and control efficiency test
Thiophene worm amine soluble granule performance indications see Table 1.
Table 1 thiophene worm amine soluble granule performance indications
| Project | Performance indications |
| Content | ≥1-20% |
| Dispersed | Adopt the graduated cylinder bulk method to carry out favorable dispersibility |
| Wetability | Adopt the measuring graduates test method(s), wetting time was less than 1 minute |
| Dissolubility | Carry out residue behind the 5min≤0.5%, residue≤2.O% behind the 18h by HG/T2467. 15-2003 |
| PH value | Undertaken by GB/T1601, measure PH5. 5～7.5 |
| Moisture | Adopt azeotropic method or karl Fischer method, moisture is less than 3.0% |
| Lasting foaming characteristic | Carry out foam volume≤60ml behind the Imin by HG/T2467. 5-2003 |
The thiophene worm amine synergy soluble granule sample that sieved is sealed in respectively in 12 50ml ampoule bottles, and about 20 gram samples are placed in 54 ± 2 ℃ of insulating boxs and detect analysis after two weeks of storage in every ampoule bottle, calculate heat storage resolution ratio.The heat storage stability result of the test sees Table 2.The result shows that thiophene worm amine synergy soluble granule heat storage stability is better, and heat storage resolution ratio is less than 5%.
The heat storage stability test of table 2 thiophene worm amine soluble granule
| Numbering | 20100801 | 20100804 | 20100809 | 20010813 | 20100815 |
| Resolution ratio, % | 1. 76 | 2. 85 | 1. 42 | 0.97 | 2. 68 |
Carry out the test of pesticide effectiveness of contact angle and cotton aphid with sample 1～4, and carry out the following of the same terms with 50% thiophene worm amine water dispersible granules and oppose than test, result of the test sees Table 3.Table 3 data show that product of the present invention is that the drug effect of comparative sample 50% thiophene worm amine water dispersible granules improves 1.4-1.5 times at the drug effect of cotton aphid, has improved the availability of active ingredient.
The synergy soluble granule control efficiency of table 3 thiophene worm amine
Claims (9)
1. thiophene worm amine synergy soluble granule, be made up of following component by weight percentage: thiophene worm amine 1～20, dispersant 1～10, wetting agent 1～5, binding agent 2～4, stabilizing agent 1～3, synergist 1～3, surplus are filler.
2. thiophene worm amine synergy soluble granule according to claim 1, it is characterized in that: described dispersant is sodium lignin sulfonate, sodium methylene bis-naphthalene sulfonate, fatty alcohol-polyoxyethylene ether or aliphatic alcohol sodium sulfate.
3. thiophene worm amine synergy soluble granule according to claim 1 is characterized in that: described wetting agent is for to methoxyl group fatty acyl amido benzene sulfonic acid sodium salt, lauryl sodium sulfate or sodium butylnaphthalenesulfonate.
4. thiophene worm amine synergy soluble granule according to claim 1, it is characterized in that: described binding agent is dextrin, polyethylene glycol or gelatin.
5. thiophene worm amine synergy soluble granule according to claim 1, it is characterized in that: described synergist is Escin, capsaicine, Butacide or triphenyl phosphate.
6. thiophene worm amine synergy soluble granule according to claim 1, it is characterized in that: described filler is maltose, glucose, soluble starch, Lactis Anhydrous or anhydrous sodium sulfate.
7. thiophene worm amine synergy soluble granule according to claim 1, it is characterized in that: described stabilizing agent is tbp or sodium hydrogen phosphate.
8. the preparation method of each described thiophene worm amine synergy soluble granule of claim 1 ~ 7, process is:
⑴ carry out coarse crushing with thiophene worm amine, dispersant, wetting agent, stabilizing agent, synergist and filler;
With coarse crushing after each component mix, carry out ultra-fine air-flow and pulverize, obtain the superfines of particle diameter below 15 microns;
⑶ add binding agent and carry out granulation;
⑷ sieve with vibratory sieve;
⑸ oven dry makes the soluble granule product.
9. the preparation method of described thiophene worm amine synergy soluble granule according to Claim 8, it is characterized in that: described bake out temperature is 60 ± 5 ℃, drying time is 1～2 hour.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103636633A (en) * | 2013-11-26 | 2014-03-19 | 广西安泰化工有限责任公司 | Application of starch as pesticide padding |
| CN104824012A (en) * | 2015-05-06 | 2015-08-12 | 河北威远生化农药有限公司 | Clothianidin synergetic patch and preparation method thereof |
| CN106518492A (en) * | 2016-10-31 | 2017-03-22 | 广东中迅农科股份有限公司 | Clothianidin granule and preparing method thereof |
| CN106857653A (en) * | 2017-02-15 | 2017-06-20 | 华北制药集团爱诺有限公司 | Soluble granule and its application process for preventing and treating root disease |
| CN107889827A (en) * | 2017-10-25 | 2018-04-10 | 江苏腾龙生物药业有限公司 | A kind of 50% clothianidin wettable powder |
| CN110519986A (en) * | 2016-09-16 | 2019-11-29 | 阿伦·沙旺特 | The stabilization formulations of water sensitivity active matter |
| CN113647386A (en) * | 2021-09-16 | 2021-11-16 | 江苏功成生物科技有限公司 | Sanitary insecticidal granules and application thereof |
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| JP2011201780A (en) * | 2010-03-01 | 2011-10-13 | Sumika Enviro-Science Co Ltd | Water-soluble insecticide granule |
| CN102388886A (en) * | 2011-10-12 | 2012-03-28 | 发事达(南通)化工有限公司 | Brassinolide water soluble granules and preparation process thereof |
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| 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 |
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Non-Patent Citations (1)
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| MIAO-FAN CHEN ET AL: "Analysis of Insecticide Clothianidin and Its Metabolites in Rice by Liquid Chromatography with a UV Detector", 《JOURNAL OF FOOD AND DRUG ANALYSIS》, vol. 13, no. 3, 31 December 2005 (2005-12-31), pages 279 - 1 * |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103636633A (en) * | 2013-11-26 | 2014-03-19 | 广西安泰化工有限责任公司 | Application of starch as pesticide padding |
| CN103636633B (en) * | 2013-11-26 | 2015-12-02 | 广西安泰化工有限责任公司 | Starch is as the application of agricultural chemicals filler |
| CN104824012A (en) * | 2015-05-06 | 2015-08-12 | 河北威远生化农药有限公司 | Clothianidin synergetic patch and preparation method thereof |
| CN104824012B (en) * | 2015-05-06 | 2017-07-07 | 河北威远生化农药有限公司 | A kind of clothianidin synergistic patch and preparation method thereof |
| CN110519986A (en) * | 2016-09-16 | 2019-11-29 | 阿伦·沙旺特 | The stabilization formulations of water sensitivity active matter |
| CN106518492A (en) * | 2016-10-31 | 2017-03-22 | 广东中迅农科股份有限公司 | Clothianidin granule and preparing method thereof |
| CN106857653A (en) * | 2017-02-15 | 2017-06-20 | 华北制药集团爱诺有限公司 | Soluble granule and its application process for preventing and treating root disease |
| CN107889827A (en) * | 2017-10-25 | 2018-04-10 | 江苏腾龙生物药业有限公司 | A kind of 50% clothianidin wettable powder |
| CN113647386A (en) * | 2021-09-16 | 2021-11-16 | 江苏功成生物科技有限公司 | Sanitary insecticidal granules and application thereof |
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| CN103238617B (en) | 2015-01-28 |
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