CN102475084A - Methylamino abamectin benzoate water dispersible granules and method for preparing same - Google Patents

Methylamino abamectin benzoate water dispersible granules and method for preparing same Download PDF

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Publication number
CN102475084A
CN102475084A CN2010105606255A CN201010560625A CN102475084A CN 102475084 A CN102475084 A CN 102475084A CN 2010105606255 A CN2010105606255 A CN 2010105606255A CN 201010560625 A CN201010560625 A CN 201010560625A CN 102475084 A CN102475084 A CN 102475084A
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China
Prior art keywords
emamectin
benzoate
dispersible granules
water dispersible
wetting agent
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Pending
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CN2010105606255A
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Chinese (zh)
Inventor
冯镇泰
华纯
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SHANGHAI NONGLE BIOLOGICAL PRODUCT CO Ltd
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SHANGHAI NONGLE BIOLOGICAL PRODUCT CO Ltd
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Priority to CN2010105606255A priority Critical patent/CN102475084A/en
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Abstract

The invention relates to methylamino abamectin benzoate water dispersible granules and a method for preparing the same. Raw materials include, by weight, 5-50 parts of methylamino abamectin benzoate, 1-15 parts of dispersant, 1-10 parts of wetting agent, 1-10 parts of disintegrant and 2-80 parts of filler. The raw materials are weighed, mixed well and evenly crushed in a jet mill, water is added before mixture is kneaded to lumps extruded for granulation, granules extruded are placed in a drying box to be dried, and finally the finished products are obtained by shaping and screening. Compared with the prior art, the methylamino abamectin benzoate water dispersible granules have the advantages of no dust, high content of active ingredients, proneness to disintegration in water, high dispersibility, high suspendability and the like.

Description

Emamectin-benzoate water dispersible granules and preparation method thereof
Technical field
The present invention relates to novel form agricultural chemical insecticide field, especially relate to a kind of emamectin-benzoate water dispersible granules and preparation method thereof.
Background technology
Emamectin-benzoate (Methylamino Abamectin Benzoate is called for short first dimension salt) is the macrolide disaccharide compounds that is got by AVM warp half chemosynthesis.Compare with AVM, this toxicity of compound be its 1/3rd, activity has improved 10-1000 doubly, has efficient, wide spectrum, low toxicity, noresidue, does not have advantages such as cross tolerance with other desinsection anthelmintics, is considered to the desirable substitute products of high malicious insecticide.At present, the emamectin-benzoate insecticide is in developed country's extensive use.
Emamectin-benzoate is the effect that strengthens neurotransmitter to the mechanism of action of insect, thereby makes a large amount of chlorions get into nerve cell, makes its forfeiture normal function; Show as insect and stop feed in several hours, paralysis is until death.The mode of action of emamectin-benzoate is main with stomach toxicity, has action of contace poison concurrently.
Emamectin-benzoate has high activity to a lot of insects; Especially to Lepidoptera, diptera, Homoptera, coleoptera and thrips insect super-high-efficient, has high activity like red tape leaf roller, tobacco budworm, beet armyworm, the greedy noctuid in nonirrigated farmland, cabbage looper, cabbage looper, maduca sexta, diamond-back moth, phyllocnistis citrella stainton, prodenia litura, tomato hawkmoth, potato bug, cabbage heart snout moth's larva, rice leaf folder, striped rice borer, paddy stem borer, cotton bollworm, pear sucker, peach fruit borer and aphid etc.; In addition, emamectin-benzoate has high activity to mite pest, like citrus red mite, European red mite, cotton red spider, apple Tetranychus urticae etc.Since the broad spectrum activity of emamectin-benzoate desinsection, and be difficult for making insect to develop immunity to drugs, and the insect that other agricultural chemicals has been produced resistance is still effective, thereby is also used more and more widely at home.
At present, domestic emamectin-benzoate preparation is main with missible oil and microemulsion, contain in the preparation a large amount of toluene, xylol, methyl alcohol to human health and the influential organic solvent of environment.Missible oil and microemulsion formulation are not only unfriendly to environment, and because petroleum price rise increases the production cost of raw material.In addition, missible oil and microemulsion formulation are that liquid state is not easy to packing, storage and transportation, so the development of new preparation has been trend of the times to substitute missible oil and microemulsion formulation.
Water dispersible granules (water dispersible granule, be called for short WDG) is a kind of pesticides new formulation that developed country such as America and Europe grows up on the basis of wetting powder and suspending agent.
Water dispersible granules mainly is made up of pesticide active ingredient, dispersant, wetting agent, binding agent, disintegrant and carrier, particle diameter 200 μ m-5mm, and disintegration rapidly after the entry disperses, and forms the higher suspension dispersion.
Summary of the invention
The object of the invention is exactly for the defective that overcomes above-mentioned prior art existence a kind of emamectin-benzoate water dispersible granules that does not have dust, active constituent content height, good dispersion and preparation method thereof to be provided.
The object of the invention can be realized through following technical scheme:
The emamectin-benzoate water dispersible granules is characterized in that, this dispersible granule comprises following component and weight portion content:
Emamectin-benzoate 5~50;
Dispersant 1~15;
Wetting agent 1~10;
Disintegrant 1~10;
Filler 2~80.
Described dispersant is one or more in polycarboxylate salt dispersant, anionic sulphonate or the block copolymer.
Described anionic sulphonate is an alkylsulfonate, comprise Akzo Nobel N.V. dispersant D500 or D425; Described block copolymer comprises the Pluronic PE of BASF AG, the Efka4300 of EFKA chemical company and the Elvacite series dispersant of Efka4330 or Du Pont company.
Described wetting agent is one or more in alkyl sulfonates wetting agent, anion wetting agent or the alkylaryl sodium naphthalene sulfonate.
Described alkyl sulfonates wetting agent comprises the TERWET 1004 of HUNTSMAN company, and described anion wetting agent comprises the wetting agent Morwet EFW of Akzo Nobel N.V..
Described disintegrant is one or more in sodium carbonate, laminated crystal of sodium disilicate or the soluble starch.
Described filler is one or more in kaolin, precipitated calcium carbonate or the diatomite.
The preparation method of emamectin-benzoate water dispersible granules is characterized in that, this method may further comprise the steps:
(1) get the raw materials ready according to following component and weight portion content:
Emamectin-benzoate 5~50,
Dispersant 1~15,
Wetting agent 1~10,
Disintegrant 1~10,
Filler 2~80;
(2) take by weighing emamectin-benzoate, wetting agent, dispersant, disintegrant and filler according to proportioning, place mixer to mix the back and evenly pulverize at airslide disintegrating mill;
(3) add entry in the material after pulverizing, in agitator, mediate then, make material be agglomerated into piece, kneaded material is used the Squeezinggranulator extruder grain;
(4) particle of extruding is placed baking oven inner drying 8~10h, the control oven temperature carries out shaping and promptly obtains product with screening at 50~55 ℃ after the drying.
The addition of the water described in the step (3) is 10~15wt% of the material after pulverizing.
Compared with prior art, the present invention has the following advantages:
(1) solved the percutaneous toxicity of missible oil, no dust to operator's safety, has also reduced the pollution to environment simultaneously;
(2) compare with other formulations, the WDG active constituent content is high, helps the agricultural chemicals decrement and uses;
(3) the product relative density is big, and volume is little, give packing, transportation, store and bring very big economy and society benefit, and packing material is easy to handle;
(4) entry easy disintegrating, good dispersion, suspensibility is high, makes utilization rate of active components improve greatly;
(5) suspension is good again, and the soup for preparing did not use up the same day, and second day warp stirs and can suspend again, do not influence application;
(6) to some unsettled former medicines in water, it is good than suspending agent etc. to process the WDG effect.
Embodiment
Below in conjunction with specific embodiment the present invention is elaborated.
Embodiment 1
The preparation method of emamectin-benzoate water dispersible granules, this method may further comprise the steps:
Prescription (wt%): emamectin-benzoate 5%, polycarboxylate salt dispersant 2%, alkyl sulfonates wetting agent 1%, sodium carbonate 1%, precipitated calcium carbonate 20%, kaolin 71%;
Operating procedure:
Successively emamectin-benzoate, polycarboxylate salt dispersant, alkyl sulfonates wetting agent, sodium carbonate, precipitated calcium carbonate and kaolin are placed in the container by above-mentioned prescription, pour in the mixer again and mix.In airslide disintegrating mill, pulverize evenly.The powder of pulverizing adds the water of 10wt%, in agitator, mediates, and makes material be agglomerated into piece.Kneaded material is used the Squeezinggranulator extruder grain.Be put in the baking oven inner drying to the particle of extruding, the control oven temperature is 54 ℃ of dryings.Carry out shaping and screening after the drying, obtain qualified product after the screening.
Embodiment 2
The preparation method of emamectin-benzoate water dispersible granules, this method may further comprise the steps:
Prescription (wt%): emamectin-benzoate 30%, polycarboxylate salt dispersant 3.5%, anion wetting agent 3.5%, laminated crystal of sodium disilicate 1%, kaolin 58.5%;
Operating procedure:
Successively emamectin-benzoate, polycarboxylate salt dispersant, anion wetting agent, laminated crystal of sodium disilicate and kaolin are placed in the container by above-mentioned prescription, pour in the mixer again and mix.In airslide disintegrating mill, pulverize evenly.The powder of pulverizing adds the water of 15wt%, in agitator, mediates, and makes material be agglomerated into piece.Kneaded material is used the Squeezinggranulator extruder grain.Be put in the baking oven inner drying to the particle of extruding.Carry out shaping and screening after the drying, obtain qualified product after the screening.
Embodiment 3
The preparation method of emamectin-benzoate water dispersible granules, this method may further comprise the steps:
Prescription (wt%): emamectin-benzoate 50%, polycarboxylate salt dispersant 10%, anion wetting agent 8%, laminated crystal of sodium disilicate 8%, kaolin 24%;
Operating procedure:
Successively emamectin-benzoate, polycarboxylate salt dispersant, anion wetting agent, laminated crystal of sodium disilicate and kaolin are placed in the container by above-mentioned prescription, pour in the mixer again and mix.In airslide disintegrating mill, pulverize evenly.The powder of pulverizing adds the water of 10wt%, in agitator, mediates, and makes material be agglomerated into piece.Kneaded material is used the Squeezinggranulator extruder grain.Be put in the baking oven inner drying to the particle of extruding.Carry out shaping and screening after the drying, obtain qualified product after the screening.
Embodiment 4
The preparation method of emamectin-benzoate water dispersible granules, this method may further comprise the steps:
(1) gets the raw materials ready according to following component and content: emamectin-benzoate 5kg, dispersant 1kg, wetting agent 10kg, disintegrant 10kg, filler 2kg; Wherein dispersant is Akzo Nobel's dispersant D-425; Wetting agent is the wetting agent Morwet EFW of Akzo Nobel N.V. and the mixture of alkylaryl sodium naphthalene sulfonate; Disintegrant is a soluble starch, and filler is a kaolin;
(2) take by weighing emamectin-benzoate, wetting agent, dispersant, disintegrant and filler according to proportioning, place mixer to mix the back and evenly pulverize at airslide disintegrating mill;
(3) water of adding 15wt% in the material after pulverizing is mediated in agitator then, makes material be agglomerated into piece, and kneaded material is used the Squeezinggranulator extruder grain;
(4) particle of extruding is placed baking oven inner drying 8h, the control oven temperature carries out shaping and promptly obtains product with screening at 55 ℃ after the drying.
Embodiment 5
The preparation method of emamectin-benzoate water dispersible granules, this method may further comprise the steps:
(1) gets the raw materials ready according to following component and content: emamectin-benzoate 50kg, dispersant 15kg, wetting agent 1kg, disintegrant 1kg, filler 80kg; Wherein dispersant is the Efka4300 of EFKA chemical company and the mixture of Efka4330; Wetting agent is the alkylaryl sodium naphthalene sulfonate; Disintegrant is the mixture of sodium carbonate and laminated crystal of sodium disilicate, and filler is precipitated calcium carbonate and diatomaceous mixture;
(2) take by weighing emamectin-benzoate, wetting agent, dispersant, disintegrant and filler according to proportioning, place mixer to mix the back and evenly pulverize at airslide disintegrating mill;
(3) add 15wt% water in the material after pulverizing, in agitator, mediate then, make material be agglomerated into piece, kneaded material is used the Squeezinggranulator extruder grain;
(4) particle of extruding is placed baking oven inner drying 10h, the control oven temperature carries out shaping and promptly obtains product with screening at 50 ℃ after the drying.

Claims (9)

1. the emamectin-benzoate water dispersible granules is characterized in that, this dispersible granule comprises following component and weight portion content:
Emamectin-benzoate 5~50;
Dispersant 1~15;
Wetting agent 1~10;
Disintegrant 1~10;
Filler 2~80.
2. emamectin-benzoate water dispersible granules according to claim 1 is characterized in that, described dispersant is one or more in polycarboxylate salt dispersant, anionic sulphonate or the block copolymer.
3. emamectin-benzoate water dispersible granules according to claim 2 is characterized in that described anionic sulphonate is an alkylsulfonate, comprise Akzo Nobel N.V. dispersant D500 or D425; Described block copolymer comprises the Pluronic PE of BASF AG, the Efka4300 of EFKA chemical company and the Elvacite series dispersant of Efka4330 or Du Pont company.
4. emamectin-benzoate water dispersible granules according to claim 1 is characterized in that, described wetting agent is one or more in alkyl sulfonates wetting agent, anion wetting agent or the alkylaryl sodium naphthalene sulfonate.
5. emamectin-benzoate water dispersible granules according to claim 4; It is characterized in that; Described alkyl sulfonates wetting agent comprises the TERWET 1004 of HUNTSMAN company, and described anion wetting agent comprises the wetting agent Morwet EFW of Akzo Nobel N.V..
6. emamectin-benzoate water dispersible granules according to claim 1 is characterized in that, described disintegrant is one or more in sodium carbonate, laminated crystal of sodium disilicate or the soluble starch.
7. emamectin-benzoate water dispersible granules according to claim 1 is characterized in that, described filler is one or more in kaolin, precipitated calcium carbonate or the diatomite.
8. the preparation method of emamectin-benzoate water dispersible granules as claimed in claim 1 is characterized in that, this method may further comprise the steps:
(1) get the raw materials ready according to following component and weight portion content:
Emamectin-benzoate 5~50,
Dispersant 1~15,
Wetting agent 1~10,
Disintegrant 1~10,
Filler 2~80;
(2) take by weighing emamectin-benzoate, wetting agent, dispersant, disintegrant and filler according to proportioning, place mixer to mix the back and evenly pulverize at airslide disintegrating mill;
(3) add entry in the material after pulverizing, in agitator, mediate then, make material be agglomerated into piece, kneaded material is used the Squeezinggranulator extruder grain;
(4) particle of extruding is placed baking oven inner drying 8~10h, the control oven temperature carries out shaping and promptly obtains product with screening at 50~55 ℃ after the drying.
9. the preparation method of emamectin-benzoate water dispersible granules according to claim 6 is characterized in that, the addition of the water described in the step (3) is 10~15wt% of the material after pulverizing.
CN2010105606255A 2010-11-25 2010-11-25 Methylamino abamectin benzoate water dispersible granules and method for preparing same Pending CN102475084A (en)

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Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102960347A (en) * 2012-12-14 2013-03-13 江苏七洲绿色化工股份有限公司 Bactericidal composition containing prothioconazole and trifloxystrobin
CN103444708A (en) * 2013-08-01 2013-12-18 广东中迅农科股份有限公司 Water dispersible granule containing chitosan
CN103858862A (en) * 2014-02-14 2014-06-18 南京善为生物科技有限公司 Environmental-friendly emamectin benzoate water-soluble powder and preparation method thereof
CN103858861A (en) * 2014-02-14 2014-06-18 南京善为生物科技有限公司 Environment-friendly emamectin benzoate aqueous solution and preparation method thereof
CN105326803A (en) * 2015-12-05 2016-02-17 翔宇药业股份有限公司 Difenidol hydrochloride tablets for treating motion sickness and preparation method thereof
CN106857569A (en) * 2016-12-23 2017-06-20 孙华飞 A kind of emamectin-benzoate mite killing suspending agent of photoactivation synergy and preparation method thereof
CN107494557A (en) * 2017-08-02 2017-12-22 江苏仁信化工有限公司 A kind of emamectin-benzoate granule and its production method
US10206402B2 (en) 2014-02-14 2019-02-19 Nanjing Scienx Biological Technology Co., Ltd. Environmentally-friendly emamectin benzoate preparation and preparation method therefor
CN112106769A (en) * 2020-09-11 2020-12-22 惠州市银农科技股份有限公司 Emamectin benzoate dry suspending agent and preparation method thereof
CN116831133A (en) * 2023-07-04 2023-10-03 山东宇润化工有限公司 Emamectin benzoate water dispersible granule and preparation method thereof

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1568695A (en) * 2003-06-27 2005-01-26 北京邦农达生物工程技术有限公司 Stable methylamino avermectin water dispersed granula
CN101361479A (en) * 2008-09-19 2009-02-11 广州市顾地丰农药有限公司 Water dispersion granule of methylamino avermectin benzoate and preparation method thereof
CN101632368A (en) * 2009-08-31 2010-01-27 江苏辉丰农化股份有限公司 Insecticidal and acaricidal composition containing emamectin benzoate
CN101632355A (en) * 2009-08-31 2010-01-27 桂林集琦生化有限公司 Pesticide water dispersible granule containing organic silicon surface active agent and preparation method thereof
CN101692808A (en) * 2009-09-30 2010-04-14 深圳诺普信农化股份有限公司 Emamectin benzoate solid lipid nanoparticle and preparation method and application thereof in pesticide formulation

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1568695A (en) * 2003-06-27 2005-01-26 北京邦农达生物工程技术有限公司 Stable methylamino avermectin water dispersed granula
CN100559944C (en) * 2003-06-27 2009-11-18 北京绿色农华生物工程技术有限公司 A kind of stable Affirm (Merck Co.) water dispersible granules
CN101361479A (en) * 2008-09-19 2009-02-11 广州市顾地丰农药有限公司 Water dispersion granule of methylamino avermectin benzoate and preparation method thereof
CN101632368A (en) * 2009-08-31 2010-01-27 江苏辉丰农化股份有限公司 Insecticidal and acaricidal composition containing emamectin benzoate
CN101632355A (en) * 2009-08-31 2010-01-27 桂林集琦生化有限公司 Pesticide water dispersible granule containing organic silicon surface active agent and preparation method thereof
CN101692808A (en) * 2009-09-30 2010-04-14 深圳诺普信农化股份有限公司 Emamectin benzoate solid lipid nanoparticle and preparation method and application thereof in pesticide formulation

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
王德平等: "甲氨基阿维菌素苯甲酸盐5%水分散粒剂的研制", 《农药科学与管理》, no. 03 *

Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102960347A (en) * 2012-12-14 2013-03-13 江苏七洲绿色化工股份有限公司 Bactericidal composition containing prothioconazole and trifloxystrobin
CN103444708A (en) * 2013-08-01 2013-12-18 广东中迅农科股份有限公司 Water dispersible granule containing chitosan
CN103858862A (en) * 2014-02-14 2014-06-18 南京善为生物科技有限公司 Environmental-friendly emamectin benzoate water-soluble powder and preparation method thereof
CN103858861A (en) * 2014-02-14 2014-06-18 南京善为生物科技有限公司 Environment-friendly emamectin benzoate aqueous solution and preparation method thereof
US10206402B2 (en) 2014-02-14 2019-02-19 Nanjing Scienx Biological Technology Co., Ltd. Environmentally-friendly emamectin benzoate preparation and preparation method therefor
CN105326803A (en) * 2015-12-05 2016-02-17 翔宇药业股份有限公司 Difenidol hydrochloride tablets for treating motion sickness and preparation method thereof
CN106857569A (en) * 2016-12-23 2017-06-20 孙华飞 A kind of emamectin-benzoate mite killing suspending agent of photoactivation synergy and preparation method thereof
CN107494557A (en) * 2017-08-02 2017-12-22 江苏仁信化工有限公司 A kind of emamectin-benzoate granule and its production method
CN112106769A (en) * 2020-09-11 2020-12-22 惠州市银农科技股份有限公司 Emamectin benzoate dry suspending agent and preparation method thereof
CN116831133A (en) * 2023-07-04 2023-10-03 山东宇润化工有限公司 Emamectin benzoate water dispersible granule and preparation method thereof
CN116831133B (en) * 2023-07-04 2024-04-26 山东宇润化工有限公司 Emamectin benzoate water dispersible granule and preparation method thereof

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Application publication date: 20120530