CN103518712B - Sustained-release chloroacetamide herbicide water dispersible granule and preparation method thereof - Google Patents
Sustained-release chloroacetamide herbicide water dispersible granule and preparation method thereof Download PDFInfo
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- CN103518712B CN103518712B CN201310520397.2A CN201310520397A CN103518712B CN 103518712 B CN103518712 B CN 103518712B CN 201310520397 A CN201310520397 A CN 201310520397A CN 103518712 B CN103518712 B CN 103518712B
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Abstract
The invention discloses a sustained-release chloroacetamide herbicide water dispersible granule and a preparation method thereof, which belongs to the field of pesticide preparations. The method comprises the following concrete steps: mixing a chloroacetamide herbicide with an aqueous solution of an alkyl quaternary ammonium salt cationic emulsifier and carrying out sufficient stirring or mixing until a partially emulsified emulsion is formed; then successively adding bentonite, a dispersant, a wetting agent, a disintegrating agent and a stabilizing agent and carrying out uniform stirring and high shear emulsification so as to obtain a herbicide suspension; and finally carrying out spray drying so as to prepare the water dispersible granule. With the method provided by the invention, the water dispersible granule with good suspension properties and a sustained-release effect is prepared, and the water dispersible granule has the advantages of convenience in processing, good security and the like and is beneficial for improving the utilization rate of pesticides and mitigating pollution of pesticides to the environment.
Description
Technical field
The invention belongs to field of pesticide preparation, particularly relate to a kind of sustained-release chloroacetamide herbicide water dispersible granule and preparation method thereof.
Background technology
In order to improve Pesticide use safety, control agricultural chemicals to the adverse effect of ecotope, with water dispersible granules etc. for the novel agrochemical formulations development in recent years of representative is rapid.Relative to Traditional Agricultural pharmaceutically dosage forms such as missible oil, water dispersible granules tool has the following advantages: 1) use Shi Yishui as dispersion medium, and not with an organic solvent, Environmental compatibility is good; 2) fater disintegration and then form suspension in water, can Direct spraying, and use conveniently, without problems such as dust from flying, safety is higher; 3) active component content is high, and packaging volume is little, and storing and transporting security is convenient; 4) better stability of preparation, formulation strong adaptability, is applicable to liquid, the former medicine of solid, also goes for the pesticide activity component that in water, solvability is higher.
At present, the preparation technology of water dispersible granules mainly comprise mixing, pulverize or grinding, granulation, drying and other steps.Moulding process has extruder grain, spray drying granulation etc., adds a small amount of binding agent sometimes to improve molding effect.Although prior art can solve water dispersant some problems in shaping and serviceability, but, pesticide activity component release in most water dispersible granules is very fast, after using, active component easily to move both vertically leaching loss with the loss of surface runoff or with soil moisture, causes agricultural chemicals availability lower and polluted surface or body of groundwater.Adopt the rate of release of slow release method reasonable adjusting pesticide activity component, thus improve drug effect, prolongation lasting period.Meanwhile, agricultural chemicals migration in the environment can be reduced, control pesticide pollution from source.
Microcapsule formulations is a kind of slow-release pesticide preparation technique.In this technology, first former medicine is dispersed into microlayer model, then with the macromolecular compound such as Lauxite parcel, forms bag in film and carry the capsule structure of active component, along with active component to reach the object of slowly-releasing to external diffusion through membranous wall during use.But microcapsule formulations technique is comparatively complicated, production cost is higher, and in capsule-core, often adopt part organic solvent to disperse former medicine.Therefore, be necessary development & production technique is simple, Environmental compatibility is good new sustained release preparation and technology of preparing thereof, and with the novel form combine with technique such as water dispersible granules, promote China's pesticidal preparations industrial expansion.
At present, there is not yet the report to chloro-acetamide herbicide water dispersible granule in existing document.
Summary of the invention
The object of this invention is to provide a kind of sustained-release chloroacetamide herbicide water dispersible granule, it is good and have the herbicide water dispersible granule of slow releasing function that the inventive method can obtain settling flux, there is the advantages such as easy to process, preparation security is good, be conducive to improving agricultural chemicals availability, alleviating the pollution of agricultural chemicals to environment.
In order to achieve the above object, the present invention is solved by following technical proposals:
Sustained-release chloroacetamide herbicide water dispersible granule, is by chloro-acetamide weed killer herbicide and alkyl quaternary ammonium salts cationic emulsifier aqueous solution, fully stirs or be mixed to forming section emulsion; Then add bentonite, dispersant, wetting agent, disintegrant, stabilizing agent successively, thin up, through high-shear emulsifying after stirring, obtain Herbicidal suspension, more spray-dried obtained herbicide water dispersible granule.
The concrete preparation method of sustained-release chloroacetamide herbicide water dispersible granule is as follows:
By the aqueous solution of chloro-acetamide weed killer herbicide and alkyl quaternary ammonium salts cationic emulsifier, under normal temperature after continuous stirring or supersonic oscillations mixing 0.5-24 h, the weed killer herbicide emulsion of forming section emulsification; Add bentonite, dispersant, wetting agent, disintegrant, stabilizing agent successively, thin up, pH to 5-9 is regulated after stirring 1-24 h, through high-shear emulsifying (rotor speed 2000 more than the rpm of high-shear emulsion machine), obtain Herbicidal suspension, again spray-dried (EAT 120 DEG C ~ 160 DEG C), obtained sustained-release chloroacetamide herbicide water dispersible granule.The micella that the inventive method utilizes cationic emulsifier to be formed wraps up a part of herbicide active active ingredients, and then is adsorbed on surperficial electronegative bentonite micron particles, thus realizes the slowly-releasing to herbicide active active ingredients; Compared with existing slow release method, preparation processing is easy, safety good.
As preferably, described alkyl quaternary ammonium salts cationic emulsifier to refer on its molecular structure respectively containing the organic surface active agent that hydrophilic quaternary ammonium and carbon chain lengths are hydrophobic alkyl between 10 ~ 20, can be any one in softex kw, Cetyltrimethylammonium bromide, hexadecyltrimethylammonium chloride, bromide sixteen alkyls pyridine.Described bentonite refers to sodium montmorillonite for main component and the powdered clay mineral of granularity below 75 microns.The inventive method utilizes the hydrophily and water dispersible that bentonite micron particles is good, in conjunction with high-shear emulsifying and spraying dry, obtains the water dispersible granules that settling flux is good; Compared with existing chloro-acetamide herbicide formulations technology, preparation is safe and convenient to use, Environmental compatibility good.
As preferably, the mass ratio of described bentonite and chloro-acetamide weed killer herbicide is (0.1-2): 1; The mass ratio of dispersant and chloro-acetamide weed killer herbicide is (0.05-0.5): 1; The mass ratio of wetting agent and chloro-acetamide weed killer herbicide is (0.05-0.5): 1; The mass ratio of disintegrant and chloro-acetamide weed killer herbicide is (0.05-0.5): 1; The mass ratio of stabilizing agent and chloro-acetamide weed killer herbicide is (0.01-0.3): 1.
As preferably, described chloro-acetamide weed killer herbicide refers to the class weed killer herbicide containing chloro-acetamide construction unit on molecular structure, can be any one in Acetochlor, the third careless amine, butachlor, isopropyl methoxalamine.
As preferably, described dispersant refers to the combination of one or more of the surfactant containing anionic group (as carboxylate radical, sulfonate radical) such as lignosulfonates, naphthalene sulfonate or its formaldehyde condensation products, polycarboxylate etc.Add described dispersant to contribute to improving the dispersiveness of preparation in water and settling flux.
As preferably, described wetting agent refers in lauryl sodium sulfate equimolecular structure containing the combination that hydrophily sulfate and carbon chain lengths are one or more of the surfactant of hydrophobic alkyl between 10 ~ 16.Add described wetting agent to contribute to improving the wetting and rate of dispersion of preparation in water, to form suspension fast, easy to use.
As preferably, described disintegrant is any one or several combination in sodium sulphate, ammonium sulfate, sodium chloride.Add described disintegrant and contribute to preparation granules fater disintegration and dispersion in water, improve the homogeneity of suspension.
As preferably, described stabilizing agent refers to the water-soluble macromolecule containing hydroxyl or carboxyl in structure, can be the combination of any one or several in sodium alginate, carboxymethyl starch, sodium carboxymethylcellulose, xanthans.Add described stabilizing agent to contribute to improving the suspension stability of preparation in water, improve settling flux rate.
As preferably, the mass percent of the aqueous solution of described alkyl quaternary ammonium salts cationic emulsifier is 0.1%-10%.
As preferably, described chloro-acetamide weed killer herbicide and the mass ratio of alkyl quaternary ammonium salts cationic emulsifier are (1-50): 1.In this quality than in scope, cationic emulsifier can form micella and wrap up a part of herbicide active active ingredients, is conducive to the absorption of weed killer herbicide on bentonite micron particles, thus realizes the slowly-releasing to herbicide active active ingredients.
The method of the invention also can be used for the water dispersible granules preparation of other non-chloro-acetyl amine liquid herbicide, as prepared the water dispersible granules of the weed killer herbicides such as 2,4-D butyl ester, clomazone.The method of the invention also can be used for the Compositional type water dispersible granules of chloro-acetamide weed killer herbicide and other weed killer herbicide.
The present invention, owing to have employed above technical scheme, has significant technique effect:
(1) micella utilizing cationic emulsifier to be formed wraps up a part of herbicide active active ingredients, and then is adsorbed on surperficial electronegative bentonite micron particles, thus realizes the slowly-releasing to herbicide active active ingredients; Compared with prior art, preparation processing is easy, safety good.
(2) utilize hydrophily and water dispersible that bentonite micron particles is good, in conjunction with high-shear emulsifying and spray drying technology, obtain the water dispersible granules that settling flux is good; Compared with existing chloro-acetamide herbicide formulations technology, preparation is safe and convenient to use, Environmental compatibility good.
(3) this slow release type preparation is conducive to improving agricultural chemicals availability, alleviating the pollution of agricultural chemicals to environment.
Accompanying drawing explanation
Fig. 1 is the releasing curve diagram of embodiment 1 gained Acetochlor water dispersible granules and 50% acetochlor ec preparations. Control.
Fig. 2 releasing curve diagram that to be the careless amine water dispersible granules of embodiment 2 gained third contrast with the 50% the third careless amine cream preparations.
Embodiment
Below in conjunction with accompanying drawing 1 and accompanying drawing 2 and specific embodiment, the present invention is described in further detail:
embodiment 1
Take 5 g softex kws, add in 500 mL distilled water, be stirred to and dissolve completely.Add 30 g acetochlor tcs, continuous stirring 2 h is to forming a part of emulsion.Add 30 g bentonites, 6 g sodium lignin sulfonates, 3 g lauryl sodium sulfate, 5 g ammonium sulfate, 2 g sodium carboxymethylcelluloses according to this, add water 1000 mL dilutions, continuous stirring 5 h dissolves to auxiliary agent, is uniformly dispersed, regulate pH to 7.0, under rotating speed 10000 rpm, high-shear emulsifying is even, spraying dry (EAT 130 DEG C) collects pressed powder afterwards, obtains 76 g water dispersible granules.The efficient liquid-phase chromatography method Acetochlor content recorded in preparation is adopted to be 35.6%.Recording settling flux rate in the water of said preparation according to standard GB/T/T 14825-2006 is 91.3%.
embodiment 2
Take 5 g OTACs, add in 500 mL distilled water, be stirred to and dissolve completely.Add the former medicine of the careless amine of 20 g third, continuous stirring 6 h is to forming a part of emulsion.Add 18 g bentonites, 4 g sodium methylene bis-naphthalene sulfonates, 2 g lauryl sodium sulfate, 3 g sodium sulphate, 1.5 g sodium alginates successively, add water 800 mL dilutions, continuous stirring 8 h dissolves to auxiliary agent, is uniformly dispersed, regulate pH to 7.0, under rotating speed 12000 rpm, high-shear emulsifying is even, spraying dry (EAT 140 DEG C) collects pressed powder afterwards, obtains 51.5 g water dispersible granules.The the third careless amine content adopting efficient liquid-phase chromatography method to record in preparation is 35.0%.Recording settling flux rate in the water of said preparation according to standard GB/T/T 14825-2006 is 88.5%.
embodiment 3
In order to verify the sustained release performance of gained water dispersible granules in above-described embodiment, and contrast with conventional cream preparation (50% acetochlor ec, 50% the third careless amine missible oil), bibliography (Zhong Jiawei etc., agricultural chemicals, 2013,52 (4), 249-251) method in, has carried out the release experiment through upper soll layer.Experimental technique is as follows: be in the Buchner funnel of 8 cm at internal diameter, and tile the thick soil of 2 cm, sprays distilled water and soaks soil to saturated.After 12 h, each 10 mg of water dispersible granules of preparation in Example 1 and embodiment 2, are watered 10 mL, are evenly sprayed at soil surface.Naturally after drying 1 h, with 40 mL distilled water sprays, collect and drench fluid, adopt the herbicide active active ingredients content in efficient liquid-phase chromatography method analysis pouring fluid.Spray distilled water amounts to 9 times, every minor tick 1 h.Calculate and add up to drench the percentage that the herbicide active active ingredients content accounts for initial application total amount, be release rate (%).Draw the variation relation of release rate with spray number of times, i.e. releasing curve diagram.
Fig. 1 is the release profiles of embodiment 1 gained Acetochlor water dispersible granules and 50% acetochlor ec preparations. Control, Fig. 2 release profiles that to be the careless amine water dispersible granules of embodiment 2 gained third contrast with the 50% the third careless amine cream preparations.As can be seen from Fig. 1, Fig. 2, compared with cream preparation, after identical spray number of times, the release rate of each group water dispersible granules obviously declines, and embodies gained water dispersible granules of the present invention comparatively slow to the release of herbicide active active ingredients, namely has obvious sustained release performance.
In a word, the foregoing is only preferred embodiment of the present invention, all equalizations done according to the present patent application the scope of the claims change and modify, and all should belong to the covering scope of patent of the present invention.
Claims (10)
1. the preparation method of sustained-release chloroacetamide herbicide water dispersible granule, is characterized in that, method is as follows:
By the aqueous solution of chloro-acetamide weed killer herbicide and alkyl quaternary ammonium salts cationic emulsifier, under normal temperature after continuous stirring or supersonic oscillations mixing 0.5-24 h, the weed killer herbicide emulsion of forming section emulsification; Add bentonite, dispersant, wetting agent, disintegrant, stabilizing agent successively, thin up, stirs 1-24 h and evenly regulates pH to 5-9 afterwards, through high-shear emulsifying, obtain Herbicidal suspension, more spray-dried obtained sustained-release chloroacetamide herbicide water dispersible granule.
2. the preparation method of sustained-release chloroacetamide herbicide water dispersible granule according to claim 1, is characterized in that: described alkyl quaternary ammonium salts cationic emulsifier is any one or several combination in softex kw, Cetyltrimethylammonium bromide, hexadecyltrimethylammonium chloride, bromide sixteen alkyls pyridine.
3. the preparation method of sustained-release chloroacetamide herbicide water dispersible granule according to claim 1, is characterized in that: the mass ratio of described bentonite and chloro-acetamide weed killer herbicide is (0.1-2): 1; The mass ratio of dispersant and chloro-acetamide weed killer herbicide is (0.05-0.5): 1; The mass ratio of wetting agent and chloro-acetamide weed killer herbicide is (0.05-0.5): 1; The mass ratio of disintegrant and chloro-acetamide weed killer herbicide is (0.05-0.5): 1; The mass ratio of stabilizing agent and chloro-acetamide weed killer herbicide is (0.01-0.3): 1.
4. the preparation method of the sustained-release chloroacetamide herbicide water dispersible granule according to claim 1 or 3, is characterized in that: described chloro-acetamide weed killer herbicide is any one in Acetochlor, the third careless amine, butachlor, isopropyl methoxalamine.
5. the preparation method of the sustained-release chloroacetamide herbicide water dispersible granule according to claim 1 or 3, is characterized in that: described dispersant is any one or several in lignosulfonates, naphthalene sulfonate or its formaldehyde condensation products, polycarboxylate.
6. the preparation method of the sustained-release chloroacetamide herbicide water dispersible granule according to claim 1 or 3, is characterized in that: described disintegrant is any one or several combination in sodium sulphate, ammonium sulfate, sodium chloride.
7. the preparation method of the sustained-release chloroacetamide herbicide water dispersible granule according to claim 1 or 3, is characterized in that: described stabilizing agent is the combination of any one or several in sodium alginate, carboxymethyl starch, sodium carboxymethylcellulose, xanthans.
8. the preparation method of sustained-release chloroacetamide herbicide water dispersible granule according to claim 1, is characterized in that: the mass percent of the aqueous solution of described alkyl quaternary ammonium salts cationic emulsifier is 0.1%-10%.
9. the preparation method of sustained-release chloroacetamide herbicide water dispersible granule according to claim 1, is characterized in that: described chloro-acetamide weed killer herbicide and the mass ratio of alkyl quaternary ammonium salts cationic emulsifier are (1-50): 1.
10. one kind as arbitrary in claim 1-9 as described in the sustained-release chloroacetamide herbicide water dispersible granule for preparing of method.
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| CN106212481A (en) * | 2016-07-26 | 2016-12-14 | 江苏省农用激素工程技术研究中心有限公司 | Flufenacet water dispersible granules and preparation method thereof |
| CN109392904A (en) * | 2018-12-03 | 2019-03-01 | 黄美红 | A kind of efficiently quickly disintegrated cell member herbicide |
| CN109575144B (en) * | 2018-12-03 | 2021-07-02 | 济南天邦化工有限公司 | Quaternary ammonium-sulfonated microcrystalline cellulose stabilizer and application thereof in cytometaherbicide |
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| TWI305134B (en) * | 2003-01-23 | 2009-01-11 | Nippon Soda Co | Agricultural and horticultural granular water-dispersible powder |
| CN101273718A (en) * | 2008-04-09 | 2008-10-01 | 绍兴文理学院 | Pesticides gel preparations for delaying release of pesticides and method for preparing the same |
| CN101278671A (en) * | 2008-04-09 | 2008-10-08 | 绍兴文理学院 | Plural gel preparation for delaying release of herbicide and method of preparing the same |
| CN102217595B (en) * | 2011-04-20 | 2013-09-25 | 绍兴文理学院 | Phytocide granule and preparation method of granule |
| CN102939961B (en) * | 2012-11-06 | 2014-07-30 | 绍兴文理学院 | Pesticide microparticle preparation having core-shell structure and preparation method thereof |
| CN102939960B (en) * | 2012-11-06 | 2014-07-02 | 绍兴文理学院 | Sustained-release herbicide microparticle preparation and preparation method thereof |
| CN103109817B (en) * | 2013-03-11 | 2014-11-05 | 叶长东 | Weeding composition containing ametryn and acetochlor |
| CN103283730A (en) * | 2013-05-22 | 2013-09-11 | 吴江市德佐日用化学品有限公司 | Weeding composition for corn field |
| CN103348981B (en) * | 2013-07-31 | 2015-03-25 | 河北博嘉农业有限公司 | Paddy field herbicide compounded with benzobicylon |
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