CN101455196B - Pesticide effervescence combination and preparation method thereof - Google Patents

Pesticide effervescence combination and preparation method thereof Download PDF

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Publication number
CN101455196B
CN101455196B CN200810044166A CN200810044166A CN101455196B CN 101455196 B CN101455196 B CN 101455196B CN 200810044166 A CN200810044166 A CN 200810044166A CN 200810044166 A CN200810044166 A CN 200810044166A CN 101455196 B CN101455196 B CN 101455196B
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pesticide
effervescence
water
agricultural chemicals
acid
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CN101455196A (en
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孙锦程
郝蕙玲
巴剑波
林永丽
武文斌
徐雄利
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Navy Medicine Research Institute of PLA
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Navy Medicine Research Institute of PLA
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Abstract

The invention relates to a agricultural chemicals branch of technology, specifically to an agriculture chemicals effervescence composition and a preparation method thereof.The invention discloses an agricultural chemicals effervescence composition comprising effervescence components, active compounds of agricultural chemicals, and the invention is characterized in that, taking the total weight as the basic reference, the agricultural chemicals effervescence composition also comprises the following components that water soluble base with a percentage by weight of 5-45% and water-soluble high molecular polymer with percentage by weight of 3-30% which form a united vector, and the active ingredients of agricultural chemicals are coated by the carrier to form a solid highly dispersed system.Every type of matters in the agricultural chemicals effervescence composition of the present invention has a better water-soluble performance, active compounds of agricultural chemicals can be highly dispersed into particles with a size of 0.001-0.1micrometre, the particle size of the active compounds of agricultural chemicals is much smaller than that of water-dispersion granulas, water dispersible powder and the like, the composition does not include any water-insoluble matters such as waterproofing agents, thinning agent and the like that are used by conventional effervescing agents, and once in water, the obtained effervescence composition is disintegrated instantly and rapidly and can be diffuse easily.Therefore, suspending particulate matters will never appear in the obtained solution, and if the prescription is reasonable, the solution will be clear and transparent; therefore, the composition can not only be used for expelling agriculture disease, but also be extensively used in the filed of expelling sanitation disease.

Description

A kind of pesticide effervescence combination and preparation method thereof
Technical field
The present invention relates to technical field of pesticide, be specifically related to a kind of pesticide effervescence combination and preparation method thereof.
Background technology
At present, China's existing formulation in agricultural chemicals market mainly contains wetting powder, missible oil, microemulsion etc., and these formulations exist production technology simple mostly, and production process is poor to personal security property, and is seriously polluted to production environment; Defectives such as the while is measured inconvenience in application, drug effect is relatively poor, and the agricultural chemicals availability is low, also can cause certain pollution to Agro-ecology and environment thereof, and the residue of pesticide problem is comparatively serious.Since twentyth century the nineties, the exploitation of world's pesticide new variety transforms to environmentally safe kind from the high-efficiency low-toxicity kind; Novel form and new method for using pollution-free, laborsavingization have become the important directions that the formulations of pesticide develop.After getting into Construction Technologies in Twenty-one Century, this requirement is just more urgent, water dispersible granules, does that emerging aqua type pesticidal preparations such as outstanding agent, effervescent agent occur in succession and increase of production is rapid, has much the gesture of catching up from behind.Wherein, effervescent agent is met effervesce disintegration rapidly behind water because of it, evenly diffusion, have effective, easy to use, save labor, advantage such as Environmental security, extremely the market parent looks at, the existing report of related patent U.S. Patent No..
Because most of agricultural chemicals all are water-insoluble, how to improve the key that the solvability (or dispersity) of pesticide active ingredient in water has become the preparation effervescent agent.The main solution route of existing patent is the refinement that realizes the agricultural chemicals diameter of particle through physical methods such as comminution by gas stream, perhaps can provide the adsorptive support of high surface area to realize the high degree of dispersion of active ingredient very much through adding.Like the preparation method of the disclosed one type of water-dispersible pesticide effervescent tablet of CN1947504A, mainly be with mixing granulation, compressing tablet behind each component comminution by gas stream to 500~1000 order fine powders; And CN1283388A discloses a kind of effervescent table as agricultural chemical and method for making thereof; Include adsorptive supports such as zeolite, silicic acid, white carbon, alundum (Al, diatomite in its preparation; Thereby effectively improved the dispersity of agricultural chemicals in water, the suspension of the disease that can obtaining after preparation drops in the water is used for spraying prevents and treats agricultural production, worm, crop smothering.These technical methods have improved the solubility property of agricultural chemicals in water to a certain extent; Even but comminution by gas stream reaches 1000 purpose grain diameters also still is 10 micron number magnitudes; The flushing liquor of preparation is opaque suspension, and contains the pesticide effervescence agent of water insoluble carrier, and suspended particulate substance also clearly in the flushing liquor of its preparation; These flushing liquors are removed the evil and are prone to stay the powder mark in treatment surface as being used for health, and its range of application has received certain limitation.Therefore, a kind of comparatively desirable health of preparation is removed the evil and must reduced diameter of particle and reduce not even aspect two of water-insoluble inert carriers expansion as far as possible and study with effervescent agent.
Summary of the invention
The object of the invention to provide a kind of can be in water disintegration rapidly, and the solution that makes do not contain suspended particulate, clarification, do not stay pesticide effervescence combination of powder mark and preparation method thereof after executing.
The present invention will mainly realize through following technological means: on the one hand, high molecular weight water soluble polymer such as polyethylene glycol and water-soluble base such as carbohydrate are united as coating pesticide composition are prepared into solid solution---solid high degree of dispersion system, and the particle diameter of pesticide composition in carrier can reach 0.001~0.1 micron; Pesticide composition is by nanorize, and simultaneously simple high molecular polymer parcel pesticide composition is prone to form rich medicine district when the pesticide composition stripping and the further stripping that hinders medicine; The adding of the little Mr hydrotrope can make dissolving rapidly, has improved the dissolution rate of pesticide composition molecule, and pesticide composition is highly dispersed; Dissolution rate is higher in the water; Improve the biological effect of residual spray greatly, the use of effervescence component in addition, disintegration, the diffusion more rapid; Flushing liquor can be realized joining existing usefulness at present, has improved operating efficiency; On the other hand, replace waterproofing agents such as zeolite, silicic acid, white carbon, talcum powder, bentonite, diatomite, kaolin, precipitated calcium carbonate with water-soluble substances, do not stay the powder mark after executing as insecticides adjuvant.
For this reason, the invention discloses a kind of pesticide effervescence combination, comprise effervescence component and pesticide original medicine, its characteristic is being benchmark with the gross weight, and this pesticide effervescence combination also comprises following components in weight percentage,
Water-soluble base 5~45%
High molecular weight water soluble polymer 3~30%
The two constitutes joint vector, and pesticide activity component is overmolding to solid high degree of dispersion system by it.
Wherein, water-soluble base is one or more of carbohydrate, organic acid or urea etc.; Include but not limited to urea, succinic acid, xylitol, galactose.
High molecular weight water soluble polymer is meant a kind of hydrophilic macromolecular material; Can be water-soluble and form solution, one of include but not limited in polyvinyl alcohol, POLYPROPYLENE GLYCOL, polyacrylic acid, polyethylene glycol oxide, HPMA, polyethylene glycol (PEG) or the polyethylene pyrrolidone (PVP) or their any combinations.
In some embodiments, be benchmark with the gross weight, this pesticide effervescence combination is made up of following components in weight percentage:
Solid dispersion system 20~80%
Water soluble pesticide auxiliary agent 0~10%;
Effervescence component 20~75%;
Described joint vector load pesticide original medicine and surfactant constitute solid dispersion system, are benchmark with the gross weight, and said solid dispersion system comprises following component in percentage by weight:
Pesticide original medicine 0.05~20%;
Surfactant 0~20%;
Joint vector 10~50%.
This solid dispersion system is encapsulated in the pesticide activity component pesticide original medicine in the joint vector of macromolecular compound and water-soluble base formation with ultrafine particle or molecular state.
Wherein solid dispersion system is preferably: pesticide original medicine 0.2~10%, surfactant 1~10%, joint vector preferred 30~50%.
Surfactant of the present invention can be selected from anion surfactant and/or non-ionic surface active agent; Include but not limited to alkyl sulfate, alkylsulfonate, alkylaryl sulfonate, AEO, aliphatic alcohol polyethenoxy ether carboxylate, APES, tween, alkylphosphonate, polyoxyethylene alkyl aryl ether, gather one or more the combination in (alkylidene) glycol or the ligninsulfonate, preferred HLB value is 14 single or built surfactant.The main effect of surfactant is the biological effect of quickening the stripping of medicine and improving medicine, and the use of proper amount of surfactant can make the medicine high degree of dispersion become littler crystallite of particle diameter or molecular state, improves bioavilability.
Said effervescence component comprises acid source and carbon dioxide source, and acid source can be any one or more than one the combination in citric acid, tartaric acid, fumaric acid, malic acid, water-soluble amino acids, the aluminum sulfate; Carbon dioxide source can be a kind of of carbonate or bicarbonate or its combination, like materials such as sodium carbonate, potash, sodium bicarbonate, saleratus etc.Effervescence component is preferably 40~65%.
In some embodiments, for prolonging the pot-life of product, also can carbon dioxide source be handled with 5% polyethylene glycol liquid parcel.
Pesticide original medicine among the present invention can be the composite form of one or more medicines in insecticide, miticide, invertebrate poison, bactericide, nematocide, weed killer herbicide, the plant growth regulator; Especially the high-efficiency activated material during suitable health is removed the evil; Like decis, cypermethrin, cyfloxylate etc., former powder of agricultural chemicals or former oil form all do not influence its preparation.
Insecticide: organic phosphates, carbamates, organic nitrogen amidine class, nereistoxin, ureas, pyrethroid photo-labile property pyrethroid, photostability pyrethroid, organochlorine class, Organic fluoride, vegetable insecticide, microorganism insecticide, insect growth regulator, IGR, insect behaviour regulator;
Bactericide: organic phosphates dithiocarbamates, sulfamic acid class, thiosulfonates class, trichloro-methylthio class, organophosphorus compounds, organo-arsenic class, organic tin, benzene class, heterocyclic benzimidazole, miazines, triazole type, morpholine class, azophenlyene class, pyrazoles, piperazines, quinolines, benzothiazoles, furans, inorganic fungicide, microbial bactericide;
Weed killer herbicide: amide-type, dinitroaniline, carbamates, ureas, phenols, diphenyl ether, triazine, phenoxy carboxylic acid, organic phosphates, heterocyclic, sulfonylurea, imidazolone type, selective herbicide, steriland herbicide.
Insecticide can be go out that young urea, deinsectization azoles, diflubenzuron, UC 62644, desinsection are grand, among the Cyhalothrin, cyfloxylate, tefluthrin, bifenthrin, ivermectin one or more; Miticide is Cyhalothrin, AVM, bifenthrin, azacyclotin, happyly kills among full, fenbutatin oxide, fenothiocarb, the plictran one or more; Weed killer herbicide can be metsulfuron-methyl, chlorsulfuron, tribenuron-methyl, triasulfuron, thiophene methyl, ethyl methyl, benzyl ethyl methyl, surely kill, among fixed, the happy spirit of quinoline of clean, the quinclorac of fluazifop-p-butyl, Dicamba, the wealthy pleasure of gram, prowers, thiameturonmethyl, broad-leaved, fluorine grass one or more; Bactericide can be one or more among the mould prestige of second, thiophanate, triazolone, alkene azoles alcohol, nitrile bacterium azoles, propiconazole, Flusilazole, the carboxin; Plant growth regulator can be: one or more among heteroauxin, indolebutyric acid, kinetin, paclobutrazol, maleic hydrazide, alar-85, naa, chlormequat, Lodging-proof agent, inabenfide, ethrel, triacontanol, the gibberellin.
In some embodiments, said pesticide effervescence combination is a benchmark with the gross weight, also comprises the water soluble pesticide auxiliary agent 0~10% of following percentage by weight; Said water soluble pesticide auxiliary agent can be diversion agent and/or disintegrant.
The purpose that adds the diversion agent is in order to make granule break down into more granule rapidly, thereby improves disintegration rate; And the adding of disintegrant can make water become swelling action to infiltrate in the granule through wicking, can include but not limited to microcrystalline cellulose, alginic acid, carboxyrnethyl starch sodium, sodium cellulose glycolate, hydroxypropyl cellulose and the water-soluble common solid formulation disintegrant of ability.Common starch or cellulose base disintegrant are inappropriate for spraying, because they generally form gel on 50 order nozzles sieve, directly sow but can be used for paddy rice.
In some embodiments, said pesticide effervescence combination can be forms such as granule, pill, tablet.
On the other hand, the invention also discloses the preparation method of said pesticide effervescence combination, comprise the following steps:
(1) acid source, the carbon dioxide source in each component of joint vector, insecticides adjuvant and the effervescence component in will filling a prescription carries out after the ultramicro grinding subsequent use respectively;
(2) high molecular polymer and water-soluble base are mixed, be modulated into thick liquid with alcohol or ketone organic solvent at 60~75 ℃; Join pastel high speed emulsification pretreatment 10~30min, rotating speed 1000~3000r/min after pesticide original medicine, surfactant fully dissolved with a small amount of alcohol or ketone; The mixed material crushed after being dried sieved promptly get agricultural chemicals solid high degree of dispersion system;
(3) the agricultural chemicals solid dispersion system is added effervescence component, insecticides adjuvant mixing, make this pesticide effervescence combination.
The present invention compares than prior art, has following distinguishing feature:
1. has no waterproofing agent in the composition.Generally the curing of liquid pesticidal often adopts porous materials such as zeolite, silicic acid, white carbon, talcum powder, alundum (Al, bentonite, diatomite, kaolin, precipitated calcium carbonate as carrier or dilution when the agent of preparation pesticide effervescence; Composition among the present invention does not include any this type of water-insoluble; Thereby; To not have the existence of these suspended particulates in the flushing liquor that makes, satisfied the health requirement that residual spray leaves no trace of removing the evil well.
2. pesticide activity component is highly dispersed, and dissolution rate is higher in the water.On the one hand, water miscible high molecular polymer such as polyethylene glycol and carbohydrate are united as coating pesticide composition are prepared into solid solution---solid high degree of dispersion system, and the particle diameter of medicine in carrier can reach 0.001~0.1 micron, and medicine is by nanorize; On the other hand, simple high molecular polymer packaging medicine is prone to form rich medicine district when the medicine stripping and the further stripping that hinders medicine; The adding of the little Mr hydrotrope can make dissolving rapidly, has improved the dissolution rate of drug molecule, improves the biological effect of residual spray greatly; The use of effervescence component in addition; Disintegration, the diffusion more rapid, flushing liquor can be realized joining existing usefulness at present, has improved operating efficiency.
3. maximum characteristics of the present invention are that obtain solution can be completely achieved clarification and even transparent.Because there is not any water-insoluble, and the refinement of drug molecule height, propagation energy is high, and the accumulative crystallization chance of drug molecule is reduced, and optimization of C can realize the transparent fully of solution, has improved the scope of application of composition greatly.
All kinds of materials all have better water solubility in the pesticide effervescence combination according to the invention; The effervescent agent entry of preparation effervesce fast also forms solution stable, no suspended particulates, and disintegration is rapid, and it is faster that active ingredient spreads; Distribute more evenly, can give full play to drug effect; Easy to use, can stand on the ridge the tablet input or be thrown into Tanaka, also can tablet be put into the sprayer that is filled with water, thereby the saving of labor, no dust from flying, environmental pollution is little, and is safe in utilization; Except that agriculture deinsectization, also can be widely used in the health field of removing the evil.
Embodiment
Below in conjunction with specific embodiment, further illustrate the present invention.Should be understood that these embodiment only to be used to the present invention is described and be not used in the restriction scope of the present invention.The experimental technique of unreceipted actual conditions in the following example, usually according to normal condition, or the condition of advising according to manufacturer.Ratio and percentage are based on weight, unless stated otherwise.
The invention is not restricted to the pesticide active ingredient mentioned among the above embodiment; Adopt other different pesticide active ingredients; Utilize method of the present invention all can make the aqua type pesticide effervescence combination, said composition can be in water high degree of dispersion, form stability preferably or even transparent emulsion.
Embodiment 1 pesticide effervescence combination
The pesticide effervescence combination that the various prescriptions of table 1 are different
Figure G2008100441668D00061
1,2.0% pyrrole propyl ether effervescent
Carry out with reference to the technological process of production of the present invention.With 12.0 parts of polyvinylpyrrolidones, 6.0 parts of urea as joint vector under 70 ± 5 ℃ of conditions with an amount of ethanol stirring and evenly mixing; 2.0 part pyrrole propyl ether joins in the joint vector mixture after with the acetone fusion; Carry out the pyrrole propyl ether solid high degree of dispersion system that atomized drying can obtain behind the 2000r/min high speed shear emulsification 15min; With crossing 800 mesh sieves after 30.0 parts of tartaric acid, 42.0 parts of sodium bicarbonate ultramicro grinding, promptly get granulating behind pyrrole propyl ether solid dispersion system, tartaric acid, sodium bicarbonate and the abundant stirring and evenly mixing of hydroxypropyl cellulose after the screening.These article can be used for the control of Lepidoptera, coleoptera and dipteral insect, as press 20-40g/m 2Multiply in the water body kill mosquito children but directly put into mosquito, the depulization of can spraying of its 30 times of liquid is used.
2,4% cypermethrin effervescent
Carry out with reference to the technological process of production of the present invention.With 16.5 parts of PEG6000,20.0 parts of lactose as joint vector under 70 ± 5 ℃ of conditions with an amount of ethanol stirring and evenly mixing; 4.0 pour in the mixed liquor of joint vector the solid high degree of dispersion system that atomized drying behind the 1500r/min high speed shear emulsification 30min can obtain cypermethrin after part cypermethrin powder usefulness, 6.5 parts of NPEs, proper amount of acetone are fully dissolved into; 23.0 parts of tartaric acid, 32.0 parts are crossed 800 mesh sieves after with the sodium bicarbonate-PEG coating ultramicro grinding of 5%PEG6000 parcel, can obtain 4% cypermethrin effervescent granulating behind cypermethrin solid dispersion system, tartaric acid, the abundant stirring and evenly mixing of sodium bicarbonate.Get the 10.0g effervescent during use and put into the residual spray liquid that wipes out the flies and mosquitoes that can be mixed with 0.4g/L in the 1L water, the lasting period can reach more than April.
3,4% Cyhalothrin effervescent tablet
Carry out with reference to the technological process of production of the present invention.With 10,000,15.5 parts of alpha-lactoses of 15.0 parts of polyethylene glycol as joint vector under 70 ± 5 ℃ of conditions with an amount of ethanol stirring and evenly mixing; 4.0 3.0 parts of part Cyhalothrins, 6.0 parts of NPEs, sodium carboxymethylcellulose are with joining behind the acetone solution in the joint vector mixture; Carry out atomized drying behind the 2000r/min high speed shear emulsification 30min and can obtain the solid high degree of dispersion system of cypermethrin; With crossing 800 mesh sieves after 23.0 parts of tartaric acid, 33.5 parts of sodium bicarbonate-PEG coating ultramicro grinding, granulation, compressing tablet behind the abundant stirring and evenly mixing of cypermethrin solid dispersion system, tartaric acid, sodium bicarbonate after the screening can be obtained agent.Getting the 5.0g effervescent tablet puts in the 500ml water; Preparation disperses back disintegration fully automatically; Form emulsion comparatively transparent, clarification, this emulsion leaves standstill 24h and still is transparence, no floating thing, suspended particulate substance under 30 ℃ of temperature; Do not have deposition yet, show that this emulsion dispersion stabilization meets the pesticidal preparations standard-required.Because the encapsulation of polymer, the lasting effect of this flushing liquor obviously are better than the aqueous emulsion of the former medicine preparation of Cyhalothrin.
4,5% Imidacloprid effervescent
Carry out with reference to the technological process of production of the present invention.With 25.5 parts of PEG6000,10.0 parts of urea as joint vector under 70 ± 5 ℃ of conditions with an amount of ethanol stirring and evenly mixing; 5.0 part Imidacloprid and 6.5 parts of AEOs join in the joint vector mixture after with acetone solution; Carry out atomized drying behind the 2000r/min high speed shear emulsification 30min and can obtain Imidacloprid solid high degree of dispersion system, granulating behind the abundant stirring and evenly mixing of Imidacloprid solid dispersion system after 19.5 parts of tartaric acid, 27.5 parts of saleratus, 6.0 parts of carboxymethylstarch are received and sieved to obtain 5% Imidacloprid effervescent.The solution of this effervescent preparation is micro emulsion white, and no suspended particulate substance and deposition can spray on paddy rice, wheat, cotton, vegetables, tobacco, potatoes and other crops, also can prevent and treat the multiple worm of control and pass crop virosis.
5,15.4% weeding effervescent agent
Carry out with reference to the technological process of production of the present invention.With 37.0 parts of urea, 5.0 parts of polyvinylpyrrolidones as joint vector; Under 70 ± 5 ℃ of conditions, add alkyl phenol benzene sulfonate, mefenacet, bensulfuron solution with organic solvent dissolution; Behind 2000r/min high speed shear emulsification 25min, carry out atomized drying and can obtain benzene benzyl solid high degree of dispersion system, granulating behind the abundant stirring and evenly mixing of benzene benzyl solid dispersion system after 9.0 parts of tartaric acid, 12.6 parts of saleratus, 10.0 parts of carboxymethylstarch are received and sieved to obtain 15.4% benzene benzyl weeding effervescent.
Embodiment 2 pesticide effervescence combination disintegrations and solution character observation
Take by weighing prepared among the embodiment 1 five kinds of effervescent agent and commercially availablely be prone to kill special effervescent tablet by working concentration preparation 500ml aqueous solution aequum, be numbered 1-6 respectively, add back in the entry and observe disintegration time and the dispersed homogeneous degree of preparation, transparency.Every group of triplicate, disintegration time are got the average of three tests, and whether dispersing uniformity test is basis for estimation with through No. two sieves, all through being qualified, otherwise are defective, and the result sees table 2.
The disintegration time of the effervescence combination that table 2 is dissimilar and dispersed homogeneous degree, transparency are observed
Figure G2008100441668D00081
Can be known that by table the aqueous solution of six kinds of preparations all can be through No. two sieves, dispersing uniformity is good, reaches the requirement of spray formulation fully; Because agricultural is removed the evil clarity of solution is not had specific (special) requirements, test formulation all can be satisfied the demand.Because the pesticide activity component in the 1-5 preparation all exists with 0.001~0.1 micron ultrafine particle even molecular state, sprays vestige even if the flushing liquor milky white also is difficult for staying, so the effervescent agent that makes according to the present invention can be widely used in the health field of removing the evil; Like 2,3 preparations, because of pesticide activity component is efficient, wide spectrum, usage amount is low, can make the solution of preparation more transparent after the interpolation certain amount of surfactant, clarify, and more can satisfy the high request that health is removed the evil.Analyze from the preparation form, effervescent has reduced production process than effervescent tablet, has practiced thrift cost, has also shortened the preparation disintegration time, is worth recommending.
The desinsection potency test of embodiment 3 effervescent agent
With 4% Cyhalothrin effervescent tablet is example:
1. get 3 of 4% Cyhalothrins among the embodiment 1, be numbered A, B, C, put into respectively in the beaker of 500ml water, treat to leave standstill 30min after the disintegration fully;
2. from three solution, get on the common ceramic tile of 1.125ml to 15cm * 15cm respectively with pipettor, and smear evenly, each solution is smeared three blocks of ceramic tiles, dries subsequent use;
3. the examination worm is a Groton bug sensitive strain adult in 2 age in week.To try worm and divide into groups, 10 every group, each 3, force the treated side that tries worm contact ceramic tile, write down the borer population of knocking down of per minute after the manual time-keeping, will all try the interior normal nursing of glass jar that worm moves to cleaning behind the 20min, inspection extremely tries borer population during 48h.
4. result's (table 3)
Table 3 effervescent tablet is to the desinsection potency test of Groton bug
Figure G2008100441668D00091
Scope of the present invention does not receive the restriction of said specific embodiments, and said embodiment is only desired also to comprise the method and the component of functional equivalent in the scope of the invention as the single example of illustrating various aspects of the present invention.In fact, except content as herein described, those skilled in the art can easily grasp multiple improvement of the present invention with reference to the description and the accompanying drawing of preceding text.Said improvement also falls within the scope of appended claims.Every piece of list of references that preceding text are mentioned is listed this paper in as a reference all in full.

Claims (13)

1. a pesticide effervescence combination comprises effervescence component and pesticide original medicine, it is characterized in that with the gross weight being benchmark, and this pesticide effervescence combination is made up of following components in weight percentage:
Solid dispersion system 20~80%,
Water soluble pesticide auxiliary agent 0~10%,
Effervescence component 20~75%;
Wherein, said solid dispersion system comprises following component in percentage by weight:
Pesticide original medicine 0.05~20%,
Surfactant 0~20%,
Joint vector 10~50%,
With the gross weight is benchmark, and said joint vector is made up of 5~45% water-soluble base of percentage by weight and 3~30% high molecular weight water soluble polymer, and pesticide original medicine is overmolding to solid dispersion system by it; Said water-soluble base is a kind of or their any combination in carbohydrate, organic acid or the urea, and said high molecular weight water soluble polymer is one of in polyvinyl alcohol, POLYPROPYLENE GLYCOL, polyacrylic acid, polyethylene glycol oxide, HPMA, polyethylene glycol or the polyethylene pyrrolidone or their any combinations; Said water soluble pesticide auxiliary agent is diversion agent and/or disintegrant.
2. pesticide effervescence combination according to claim 1 is characterized in that said water-soluble base is one of in urea, succinic acid, xylitol, the galactose or their any combination.
3. pesticide effervescence combination according to claim 1 is characterized in that said solid dispersion system is made up of the material that with the gross weight is the following percentage by weight of benchmark: pesticide original medicine 0.2~10%, surfactant 1~10%, joint vector 30~50%.
4. pesticide effervescence combination according to claim 1 is characterized in that said surfactant is anion surfactant and/or non-ionic surface active agent.
5. pesticide effervescence combination according to claim 4 is characterized in that said surfactant is one or more the combination in alkyl sulfate, alkylsulfonate, alkylaryl sulfonate, AEO, aliphatic alcohol polyethenoxy ether carboxylate, APES, tween, alkylphosphonate, polyoxyethylene alkyl aryl ether, PAG or the ligninsulfonate.
6. pesticide effervescence combination according to claim 1 is characterized in that with the gross weight being benchmark, and the percentage by weight of said effervescence component is 40~65%.
7. according to each described pesticide effervescence combination of claim 1-6; It is characterized in that said effervescence component comprises acid source and carbon dioxide source, acid source is any one or more than one the combination in citric acid, tartaric acid, fumaric acid, malic acid, water-soluble amino acids, the aluminum sulfate; Carbon dioxide source is a kind of of carbonate or bicarbonate or its combination.
8. pesticide effervescence combination according to claim 7 is characterized in that said carbon dioxide source handles with 5% polyethylene glycol liquid parcel.
9. pesticide effervescence combination according to claim 8 is characterized in that said carbon dioxide source is one of in sodium carbonate, potash, sodium bicarbonate, the saleratus.
10. pesticide effervescence combination according to claim 1 is characterized in that said pesticide original medicine is the composite form of one or more medicines in insecticide, miticide, invertebrate poison, bactericide, nematocide, weed killer herbicide, the plant growth regulator.
11. pesticide effervescence combination according to claim 1 is characterized in that said pesticide original medicine is one or more in pyrrole propyl ether, Cyhalothrin, cypermethrin, Imidacloprid, mefenacet or the bensulfuron.
12. pesticide effervescence combination according to claim 1 is characterized in that said disintegrant is one of in microcrystalline cellulose, alginic acid, carboxyrnethyl starch sodium, sodium cellulose glycolate or the hydroxypropyl cellulose.
13. the preparation method of the said pesticide effervescence combination of claim 1 comprises the following steps:
(1) acid source, the carbon dioxide source in each component of joint vector, water soluble pesticide auxiliary agent and the effervescence component in will filling a prescription carries out after the ultramicro grinding subsequent use respectively;
(2) high molecular polymer and water-soluble base are mixed, be modulated into thick liquid with alcohol or ketone organic solvent at 60~75 ℃; Join thick liquid high speed emulsification pretreatment 10~30min, rotating speed 1000~3000r/min after pesticide original medicine, surfactant fully dissolved with alcohol or ketone; The mixed material crushed after being dried sieved promptly get the agricultural chemicals solid dispersion system;
(3) the agricultural chemicals solid dispersion system is added effervescence component, water soluble pesticide auxiliary agent mixing, make this pesticide effervescence combination.
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CN102986719B (en) * 2012-12-28 2015-01-21 江苏龙灯化学有限公司 Insecticide composition containing bifenthrin and pyriproxyfen and applications thereof
CN105076184A (en) * 2014-05-12 2015-11-25 陈政忠 Household pesticide effervescent tablet and preparation method thereof
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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5516529A (en) * 1989-04-07 1996-05-14 Zellweger; Jean-Michel Granulates useful for preparing effervescent pesticide tablets
CN1146135A (en) * 1994-04-14 1997-03-26 法国赫司特先灵阿格里沃有限公司 Novel pesticide compositions and method of preparation
EP0761212A3 (en) * 1995-09-08 1997-11-12 Takeda Chemical Industries, Ltd. Effervescent composition and its production
WO1997041732A1 (en) * 1996-05-07 1997-11-13 Hiroshi Kawai Effervescent preparation for plants
CN1234176A (en) * 1999-01-15 1999-11-10 中国科学院生态环境研究中心 Effervescence farm-chemical composition and production method thereof
CN1298644A (en) * 1999-12-03 2001-06-13 陈丰喜 Herbiciding effervescent tablet for paddy rice

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5516529A (en) * 1989-04-07 1996-05-14 Zellweger; Jean-Michel Granulates useful for preparing effervescent pesticide tablets
CN1146135A (en) * 1994-04-14 1997-03-26 法国赫司特先灵阿格里沃有限公司 Novel pesticide compositions and method of preparation
EP0761212A3 (en) * 1995-09-08 1997-11-12 Takeda Chemical Industries, Ltd. Effervescent composition and its production
WO1997041732A1 (en) * 1996-05-07 1997-11-13 Hiroshi Kawai Effervescent preparation for plants
CN1234176A (en) * 1999-01-15 1999-11-10 中国科学院生态环境研究中心 Effervescence farm-chemical composition and production method thereof
CN1298644A (en) * 1999-12-03 2001-06-13 陈丰喜 Herbiciding effervescent tablet for paddy rice

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