CN102475092A - Compounded insecticidal suspension emulsion with chlorpyrifos and spirotetramat and preparation method of compounded insecticidal suspension emulsion - Google Patents
Compounded insecticidal suspension emulsion with chlorpyrifos and spirotetramat and preparation method of compounded insecticidal suspension emulsion Download PDFInfo
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- CN102475092A CN102475092A CN2010105726191A CN201010572619A CN102475092A CN 102475092 A CN102475092 A CN 102475092A CN 2010105726191 A CN2010105726191 A CN 2010105726191A CN 201010572619 A CN201010572619 A CN 201010572619A CN 102475092 A CN102475092 A CN 102475092A
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Abstract
The invention discloses a compounded insecticidal suspension emulsion with chlorpyrifos and spirotetramat and a preparation method of the compounded insecticidal suspension emulsion. The compounded insecticidal suspension emulsion comprises the following contents in percentage by weight: 2-30% of spirotetramat, 10-40% of chlorpyrifos, 5-20% of organic solvent and the balance water, and is formed by adopting the following steps of mechanical stirring, sanding and high-speed homogeneity cutting. The compounded insecticidal suspension emulsion has a stable property and a high medicine effect, and can be used for preventing injurious insects such as scale insects of oranges, cotton and apples, bemisia tabaci of vegetables, and the like. According to the invention, the compounded insecticidal suspension emulsion has the advantages that the water is used as the main dispersion medium, the pollution to the environment is small, the situations of oil deposition, sediment and the like when the compounded insecticidal suspension emulsion is stored for two years under normal temperature are not existed, the service life of a storage rack is long and is non-flammable, the storage and the transportation is safe, compared with using the spirotetramat alone, the cost is low, and the like.
Description
Technical field:
The present invention relates to insecticide, particularly relate to a kind of compound insecticidal suspension emulsion and preparation method who contains chlopyrifos and spiral shell worm ethyl ester.
Background technology:
Chlopyrifos (chlorpyrifos) is the broad spectrum insecticide of anticholinesterase; Good tagging and stomach poison function arranged; And certain stifling property is arranged, and do not inhale and osmosis in not having, the larva of the scale insect of firm hatching, aphid, mealybug, wood louse there is good control efficiency; Scale insect effect to forming wax coat is undesirable; Insect had tag, stomach toxicity and fumigation action, be one of govern-house-variety of China control vegetables, fruit tree and soil insect, become large-tonnage agricultural chemicals in the market.
Spiral shell worm ethyl ester (spirotetramat) is a kind of novel tetronic acid insecticides, has the two-way interior conductive performance of inhaling, and insecticidal spectrum is wide, and the lasting period is long.It is that fatty biosynthesis through interference insect causes larva dead, and insect receives medicine plant to death generally to need 3-5 days getting food.Because its unique mechanism of action, can prevent and treat the insect that existing insecticide is produced resistance effectively, like the sucking pest on citrus, apple, pears, the vegetable crop: scale insect, aphid, mealybug, wood louse, trialeurodes vaporariorum, thrips etc.
Though spiral shell worm ethyl ester is effective; But quick-acting is slow, and the peasant sees just medication behind the insect, thereby is later than administration time 7-10 days; And this moment, a large amount of larvas was fixed on the growth site of plant; Receive medicine plant to death generally also to need 3-5 days getting food, just can kill off the insect pests rapidly, alleviate harm as being mixed with a kind of medicament of quick-acting to use this moment.Chlopyrifos is exactly very desirable mixed medicament.
In the actual production, the single agent of chlopyrifos has been used for citrus, apple, vegetables, cotton-plant pest-insects control with the use that mixes of spiral shell worm ethyl ester list agent.But run into following several problem in actual the use: 1, the user is not sure of the best proportioning of two medicines when bucket mixes, thereby can't obtain best preventive effect, and increment uses the expenses for prevention and control height or the unreasonable adapted that are produced to make that control is not cheap; 2, the different single agent of brand chlopyrifos have different quality (the chlorpyrifos ec list agent of selling in China reaches more than 350), and this quality that makes bucket mix can not get assurance, thereby makes control efficiency to be guaranteed.
So press for the complex preparation of a kind of spiral shell worm ethyl ester of research and development and chlopyrifos, to overcome the above problems.Obtain rational composite proportioning through the biologicall test screening, make the biological effect synergy between spiral shell worm ethyl ester and the chlopyrifos reach best, both reached the effect of synergy, can reduce the usage amount of medicament again, alleviate pressure environment.To spiral shell worm ethyl ester and chlopyrifos composite dose carries out form formula research simultaneously, give full play to the biologically active that ensures two effective ingredients, and obtain excellent field efficacy, but above-mentioned work need be paid a large amount of creative works.
Summary of the invention:
The present invention is intended to solve aforementioned technical problem, and a kind of compound insecticidal suspension emulsion that contains chlopyrifos and spiral shell worm ethyl ester and preparation method thereof is provided, and to solve chlopyrifos and the composite problem of spiral shell worm ethyl ester, for producing qualified composite product industrialization technical support is provided.
Above-mentioned purpose of the present invention is to realize through following technological means.
A kind of compound insecticidal suspension emulsion that contains chlopyrifos and spiral shell worm ethyl ester provided by the present invention, contain following component by weight percentage:
Chlopyrifos 10-40%
Spiral shell worm ethyl ester 2-30%
Organic solvent 5-20%
Water surplus.
Also contain following component by weight percentage:
Emulsifier 5-12%
Cosurfactant 0-5%
Dispersant 2-6%
Wetting agent 1-3%
Antifreezing agent 0-5%
Thickener 0-3%
Antifoaming agent 0-0.4%.
The content sum of said by weight percentage chlopyrifos, spiral shell worm ethyl ester and organic solvent is not more than 65%.
The described compound insecticidal suspension emulsion that contains chlopyrifos and spiral shell worm ethyl ester, preferably contain following component by weight percentage:
Chlopyrifos 20-30%
Spiral shell worm ethyl ester 5-20%
Organic solvent 5-10%
Emulsifier 5-10%
Cosurfactant 2-4%
Dispersant 2-4%
Wetting agent 1-2%
Antifreezing agent 2-5%
Thickener 2-3%
Antifoaming agent 0.2-0.4%
Water surplus.
Said organic solvent is selected from cyclohexanone, xylol, No. 1500 solvents, No. 1800 solvents, No. 2000 solvents, amylalcohol, isooctane or its mixtures;
Described emulsifier is selected from polyoxyethylene nonylphenol ether; APES; Fat alcohol ethoxyl compound; Styryl phenyl APEO; Alkyl phenol formaldehyde resin polyoxyethylene ether; Styrene phenol formaldehyde resin APEO; The polyoxyethylene polyoxypropylene block co-polyether; The secondary octyl phenol polyethenoxy ether; Castor oil polyoxyethylene ether; Fat alcohol alkoxy compound; Tallow ethyoxyl amine salt; Starch Sodium Octenyl Succinate; Polyoxyethylene ether phosphate salt; Alkyl phosphate salt; Naphthalene sulfonate salt or its mixture;
Said cosurfactant is selected from n-butanol, isobutanol, n-octyl alcohol or its mixture;
Described wetting agent is selected from EO/PO block polyether, AEO, fat alcohol ethoxyl compound, tallow ethyoxyl ammonium salt, alkylnaphthalene sulfonate, fatty alcohol polyoxyethylene ether sulfate, acyl group glutamate.Said dispersant is selected from naphthalene sulfonic acid condensate sodium salt, phenolsulfonic acid condensation product sodium salt, methyl naphthalene sulfonate formaldehyde condensate, sodium lignin sulfonate, sodium metnylene bis-naphthalene sulfonate, acrylate homopolymer sodium salt, polymeric polycarboxylic acid salt, dioctyl sodium sulphosuccinate salt, maleic acid-acrylic acid copolymer sodium salt or its mixture;
Said antifreezing agent is selected from ethylene glycol, PEG400, propane diols, glycerine, isopropyl alcohol or its mixture;
Described thickener is selected from xanthans, Magnesiumaluminumsilicate, sodium carboxymethylcellulose, organobentonite or its mixture;
Said antifoaming agent is silicone defoaming agent, polyether antifoam agent or its mixture;
Described water is deionized water or distilled water.
The present invention also provides a kind of preparation method who contains the compound insecticidal suspension emulsion of chlopyrifos and spiral shell worm ethyl ester, and it comprises following processing step:
A. the weight ratio according to spiral shell worm ethyl ester 2-30%, chlopyrifos 10-40%, organic solvent 5-20%, water surplus takes by weighing raw material;
B. with above-mentioned raw materials mixing, sand milling, filtration;
C. filtrate gets the suspension emulsion finished product through the high speed shear homogeneous.
The raw material that described preparation method takes by weighing with weight ratio also comprises emulsifier 5-12%, dispersant 2-6%, wetting agent 1-3%, cosurfactant 0-5%, antifreezing agent 0-5%, thickener 0-3%, antifoaming agent 0-0.4%.
The present invention provides a kind of preparation method who contains the compound insecticidal suspension emulsion of chlopyrifos and spiral shell worm ethyl ester again, and it comprises following processing step:
A. the weight ratio according to spiral shell worm ethyl ester 2-30%, chlopyrifos 10-40%, organic solvent 5-20%, water surplus takes by weighing raw material respectively;
B. the spiral shell worm ethyl ester, the water that are taken by weighing are mixed sand milling, cross and to filter spiral shell worm ethyl ester suspending agent;
C. the chlopyrifos that is taken by weighing, organic solvent are mixed, be added under the high speed shear in the spiral shell worm ethyl ester suspending agent, high speed shear, mistake filter the suspension emulsion finished product.
The raw material that described preparation method takes by weighing with weight ratio also comprises emulsifier 5-12%, dispersant 2-6%, wetting agent 1-3%, cosurfactant 0-5%, antifreezing agent 0-5%, thickener 0-3%, antifoaming agent 0-0.4%.
The present invention provides a kind of preparation method who contains the compound insecticidal suspension emulsion of chlopyrifos and spiral shell worm ethyl ester again, and it comprises following processing step:
A. the weight ratio according to spiral shell worm ethyl ester 2-30%, chlopyrifos 10-40%, organic solvent 5-20%, water surplus takes by weighing raw material respectively;
B. spiral shell worm ethyl ester is processed suspending agent;
C. chlopyrifos is processed aqueous emulsion;
D. with above gained suspending agent and aqueous emulsion high speed shear, emulsifying, mistake filter suspension emulsion.
The raw material that described preparation method takes by weighing with weight ratio also comprises emulsifier 5-12%, dispersant 2-6%, wetting agent 1-3%, cosurfactant 0-5%, antifreezing agent 0-5%, thickener 0-3%, antifoaming agent 0-0.4%.
The compound insecticidal suspension emulsion that contains spiral shell worm ethyl ester and chlopyrifos provided by the present invention can solve a difficult problem that is difficult to make conventional mixture preparation between chlopyrifos and the spiral shell worm ethyl ester; Solve pesticide resistance and the lasting period problem of insect, reduce simultaneously and use spiral shell worm ethyl ester cost problem of higher separately chlopyrifos.
Chlopyrifos and the spiral shell worm ethyl ester compound insecticidal suspension emulsion outward appearance homogeneous of containing provided by the present invention; Easy mobility; Stability of emulsion is qualified; Cold and hot storage physical stability is qualified; In heat two weeks of storage under 54 ± 1 ℃ condition, chlopyrifos and spiral shell worm ethyl ester resolution ratio are all less than 5%, and storage back preparation stability of emulsion is qualified.
There are following technology of preparing difficult point in the compound insecticidal suspension emulsion and the preparation thereof that contain chlopyrifos and spiral shell worm ethyl ester: suspension emulsion is the suspend in water aqueous pesticide preparation of the outward appearance homogeneous that forms of agricultural chemicals oil droplet and solid particle, is thermodynamic unstable system.Under action of gravity, the oil droplet of suspension and solid particle can sink gradually, in addition because of there being model ylid bloom action power between oil droplet and the solid particle, being prone to attract each other and agglomeration takes place and further quickening sedimentation, produce and pile up.When piling up gently, it is denseer thick that the preparation outward appearance is the bottom, up weakens gradually; Then occur flocculation when crossing closs packing, even produce deposition or breakdown of emulsion (analysing oil) phenomenon, cause and to disperse to form the homogeneous system again.Therefore the system stability that solves preparation is one of technological difficulties of development spiral shell worm ethyl ester chlopyrifos suspension emulsion.
The present invention is the technological difficulties that solve aforementioned suspension emulsion preparation through following approach:
1. being employed in agricultural chemicals oil droplet surface has the surfactant of strong adsorption capacity, like the polyoxyethylene polyoxypropylene block co-polyether etc., forms more stable sterically hindered effect on the oil droplet surface, prevents coalescence;
2. it is composite to select suitable surfactant to carry out, and makes composite emulsifier form the higher compound interface film of mechanical strength on agricultural chemicals oil droplet surface, and interfacial film intensity is high more, is difficult for taking place coalescence when oil droplet collides each other and increases, and system is just more stable;
3. select the suitable anion auxiliary agent,, strengthen the Zeta potential gesture, make between oil droplet, electrostatic repulsion forces strengthens between solid particle, is difficult for taking place coalescence like tallow ethyoxyl amine salt, phosphates, naphthalene sulfonate salt etc.;
4. select suitable process route and technological parameter, make oil droplet and the particle grain size distribution scope is narrower, meso-position radius is less, slow down settling velocity, and significantly alleviate the Ostwald ripening phenomenon;
5. keeping under preparation good mobility and the dispersed situation; Utilize thickener regulation system viscosity such as xanthans, Magnesiumaluminumsilicate, sodium carboxymethylcellulose, organobentonite; Form tridimensional network; Support disperse phase (spiral shell worm ethyl ester, chlopyrifos) quality, and then delayed fallout, generation deposition or demulsifying phenomenon in the shelf life phase prevented;
Through lot of test, we have selected chlopyrifos and spiral shell worm ethyl ester are developed to suspension emulsion.At least contain two kinds of water-fast active ingredients in the suspension emulsion, stably being dispersed in water with solia particle and fine liquid pearl form is in the heterogeneous liquid of continuous phase, has the advantage of suspending agent and aqueous emulsion, is a kind of Water-borne modification environment-friendly type formulation.On stream; We have overcome suspension emulsion under action of gravity; The oil droplet and the solid particle that suspend can sink gradually; And between oil droplet and the solid particle under the Van der Waals force effect, and produce agglomeration even produce deposition or breakdown of emulsion (analysing oil) phenomenon, cause the key technology difficult point that can't disperse to form the homogeneous system again.Said preparation is a waterborne preparation, does not have dust in the production process, no imbedibility health risk in the use, and the while can make the preparation of high-load, for producing, promoting the use of possibility is provided.
This case is tested both appropriate proportionings of screening through a large amount of living tests, reaches the insurmountable problem of single agent of running in the production that solves cost-effectively; Again through pharmaceutical formulation screening, production technology exploitation, the product that formation can industrialization.
Through test of many times; The content sum of said by weight percentage chlopyrifos, spiral shell worm ethyl ester and organic solvent was greater than 65% o'clock; Very few because of institute's water content in the preparation, too dense thick dispersiveness and the pourability of causing of the product of being prepared is not good, unfavorable production and use; Also can too much produce unnecessary pollution to environment because of medicament in the Packaging Bottle is remaining, very few also can causing of the water yield can't make qualified formulation products in the prescription simultaneously.
The spiral shell worm ethyl ester chlorpyrifos mixture desinsection suspension emulsion that contains provided by the present invention has following characteristics under the use of reality:
1, found desirable cosolvent, emulsifier, dispersant, wetting agent and rational production method, made spiral shell worm ethyl ester can form the suspending agent system, and chlopyrifos can stably be existed with the form of small oil droplet in this system.
2, quick-acting obviously is superior to the agent of spiral shell worm ethyl ester list, has kept long advantage of spiral shell worm ethyl ester single-dose effect phase simultaneously again; Insecticidal spectrum is extensively in list agent of spiral shell worm ethyl ester and the single agent of chlopyrifos, and medicament also is able to significantly improve.
3,, when drug effect promotes, reduced the control cost, and alleviated influence environment owing to reasonable mixture ratio.
4, water reduces environmental pollution as primary solvent, and the conservation cost can be avoided the influence of international petroleum market price simultaneously again.
5, solvent-free smell to the eye nonirritant, significantly is lower than missible oil to people's dermal toxicity.
6, make and when using safety and processing cost low.
Embodiment:
In order better to understand essence of an invention, describe the technology contents of invention below in detail with regard to the better utilization instance.But content of the present invention not only is confined to this, and all changes inseparable with essence of the present invention and scope, modification, distortion or other use and use, and all is regarded as to fall within the scope of the present invention.
In the raw material: the former medicine of spiral shell worm ethyl ester (Beyer Co., Ltd); The former medicine of chlopyrifos (Zhejiang Xinnong Chemical Co.,Ltd); 240g/L spiral shell worm ethyl ester suspending agent (Beyer Co., Ltd's production), 40% chlopyrifos ME (Zhejiang Xinnong Chemical Co.,Ltd's production), cyclohexanone, xylol, No. 1500 solvents (standing grain petrochemical industry Co., Ltd in the Jiaxing City); No. 1800 solvents (Huzhou Bohai petroleum chemical industry Co., Ltd), No. 2000 solvents (big Fine Chemical Works in Gaoyou City), amylalcohol, isooctane.
The preparation of suspension emulsion
Embodiment 1:
42% reactive compound (2% spiral shell worm ethyl ester and 40.0% chlopyrifos composition): 20.0% spiral shell worm ethyl ester, EO/PO block polyether 1%, phenolsulfonic acid condensation product sodium salt 2%, acrylate homopolymer sodium salt 1.0%, ethylene glycol 2.0%, xanthans 0.3%, polyether antifoam agent 0.1%, deionized water are supplied abundant mixing; Put into high shear emulsifying agent high speed again and shear corase grind and homogeneous; Sand milling in pump to the sand mill again; Sand milling promptly gets suspending agent to certain grain size after refiltering.Contain 20.0% spiral shell worm ethyl ester in the suspending agent, D
90Particle diameter is the 3-5 micron.Again 10% 20.0% spiral shell worm ethyl ester suspending agent, chlopyrifos 40.0%, xylol 20.0%, n-butanol 3%, alkyl phenol formaldehyde resin polyoxyethylene ether 4%, fat alcohol ethoxyl compound 8.0%, ethylene glycol 3.0%, xanthans 0.1%, polyether antifoam agent 0.1%, deionized water are supplied abundant mixing; High speed shear; Emulsifying, filtration promptly make suspension emulsion, and suspension emulsion contains the reactive compound of 42% content.
Embodiment 2:
40% reactive compound (5.0% spiral shell worm ethyl ester and 35.0% chlopyrifos composition): 25.0% spiral shell worm ethyl ester, alkylnaphthalene sulfonate 1.0%, sodium lignin sulfonate 2.0%, polymeric polycarboxylic acid salt 1.0%, PEG400 2.0%, Magnesiumaluminumsilicate 0.4%, polyether antifoam agent 0.1%, deionized water 68.6% are fully mixed; Put into high shear emulsifying agent high speed again and shear corase grind and homogeneous; Sand milling in pump to the sand mill again; Sand milling promptly gets suspending agent to certain grain size after refiltering.Contain 25.0% spiral shell worm ethyl ester in the suspending agent, D
90Particle diameter is the 3-5 micron.Again 20.0% 25.0% spiral shell worm ethyl ester suspending agent, chlopyrifos 35.0%, No. 1800 solvents 10.0%, isobutanol 5%, castor oil polyoxyethylene ether 3.0%, fat alcohol alkoxy compound 3.0%, polyethylene glycol 3.0%, Magnesiumaluminumsilicate 0.3%, polyether antifoam agent 0.1%, deionized waters are mended to 100%; Fully mix; High speed shear; Emulsifying, filtration promptly make suspension emulsion, and suspension emulsion contains the reactive compound of 40% content.
Embodiment 3:
30% reactive compound (10.0% spiral shell worm ethyl ester and 20.0% chlopyrifos composition): spiral shell worm ethyl ester 40.0%, AEO 2.0%, methyl naphthalene sulfonate formaldehyde condensate 3.0%, sodium metnylene bis-naphthalene sulfonate 1.0%, propane diols 2.0%, sodium carboxymethylcellulose 0.6%, polyether antifoam agent 0.1%, deionized water 51.5% are fully mixed; Put into high shear emulsifying agent high speed again and shear corase grind and homogeneous; Sand milling in pump to the sand mill again; Sand milling promptly gets suspending agent to certain grain size after refiltering.Contain 40% spiral shell worm ethyl ester in the suspending agent, D
90Particle diameter is the 3-5 micron.Again 25.0% 40.0% spiral shell worm ethyl ester suspending agent, chlopyrifos 20.0%, No. 1500 solvents 10.0%, tallow ethyoxyl ammonium salt 3.0%, APES 4.0%, propane diols 2.0%, sodium carboxymethylcellulose 0.3%, polyether antifoam agent 0.1%, deionized waters 35.6% are fully mixed; High speed shear; Emulsifying, filtration promptly make suspension emulsion, and suspension emulsion contains the reactive compound of 30% content.
Embodiment 4:
30% reactive compound (20.0% spiral shell worm ethyl ester and 10.0% chlopyrifos composition): spiral shell worm ethyl ester 20.0%, fat alcohol ethoxyl compound 2.0%, methyl naphthalene sulfonate formaldehyde condensate 3.0%, acrylate homopolymer sodium salt 3.0%, glycerine 2.0%, xanthans 0.2%, sodium carboxymethylcellulose 0.2%, polyether antifoam agent 0.2% chlopyrifos 10.0%, No. 2000 solvents 5.0%, secondary octyl phenol polyethenoxy ether 2.0%, polyoxyethylene ether phosphate salt 2.0%, deionized waters supplied fully mix back sand milling to meso-position radius and be in the 1-5 micron; Filter main; Promptly make suspension emulsion through the high speed shear homogeneous again, suspension emulsion contains the reactive compound of 30% content.
Embodiment 5:
35% reactive compound (5.0% spiral shell worm ethyl ester and 30.0% chlopyrifos composition): spiral shell worm ethyl ester 20.0%, tallow ethyoxyl ammonium salt 2.0%, naphthalene sulfonic acid condensate sodium salt 3.0%, acrylate homopolymer sodium salt 1.0%, isopropyl alcohol 4.0%, xanthans 0.1%, organobentonite 0.1%, polyether antifoam agent 0.1%, deionized water are supplied abundant mixing; Put into high shear emulsifying agent high speed again and shear corase grind and homogeneous; Sand milling in pump to the sand mill again; Sand milling is to certain grain size; Promptly get suspending agent after refiltering, contain 20.0.% spiral shell worm ethyl ester in the suspending agent, D
90Particle diameter is the 3-5 micron.Again 25.0% 20.0% spiral shell worm ethyl ester suspending agent, chlopyrifos 30.0%, cyclohexanone 5.0%, No. 1500 solvents 10%, n-octyl alcohol 4%, alkyl phosphate salt 2.0%, starch Sodium Octenyl Succinate 3.0%, isopropyl alcohol 3.0%, xanthans 0.3%, polyether antifoam agent 0.1%, deionized waters are supplied abundant mixing; High speed shear; Emulsifying, filtration promptly make suspension emulsion, and suspension emulsion contains the reactive compound of 35% content.
Embodiment 6:
40% reactive compound (30.0% spiral shell worm ethyl ester and 10.0% chlopyrifos composition): spiral shell worm ethyl ester 30.0%, chlopyrifos 10.0%, AEO vinethene sulphate 3.0%, methyl naphthalene sulfonate formaldehyde condensate 3.0%, dioctyl sodium sulphosuccinate salt 1.0%, amylalcohol 2.0%, No. 2000 solvents 4%, polyoxyethylene nonylphenol ether 2.0%, styryl phenyl APEO 3.0%, isopropyl alcohol 4.0%, xanthans 0.5%, organobentonite 2.5%, silicone defoaming agent 0.4%, deionized waters are supplied abundant mixing; Put into high shear emulsifying agent high speed again and shear corase grind and homogeneous; Sand milling in pump to the sand mill again; Sand milling is to certain grain size; Promptly get suspension emulsion after refiltering, suspension emulsion contains the reactive compound of 40% content.
Embodiment 7:
25% reactive compound (5.0% spiral shell worm ethyl ester and 20.0% chlopyrifos composition): 25.0% spiral shell worm ethyl ester, acyl group glutamate 1.0%, maleic acid-acrylic acid copolymer sodium salt 2.0%, polymeric polycarboxylic acid salt 1.0%, PEG400 2.0%, Magnesiumaluminumsilicate 0.4%, polyether antifoam agent 0.1%, deionized water are fully mixed after supplying; Put into sand milling in the sand mill again; Till meso-position radius is in the 1-5 micron, filters and promptly get 25% spiral shell worm ethyl ester suspending agent; Chlopyrifos 25.0%, isooctane 5.0%, No. 1800 solvents 10%, isobutanol 1%, n-octyl alcohol 1%, styrene phenol formaldehyde resin APEO 3.0%, polyoxyethylene polyoxypropylene block co-polyether 3.0%, polyethylene glycol 3.0%, Magnesiumaluminumsilicate 0.3%, polyether antifoam agent 0.1%, deionized waters are supplied abundant mixing, promptly make 25% chlorpyrifos aqueous emulsion after the high speed shear emulsifying; Again 20% 25.0% spiral shell worm ethyl ester suspending agent, 80% 25% chlorpyrifos aqueous emulsion are fully mixed, and through the high speed shear homogeneous, promptly make the reactive compound that contains 25% content.
Above sample is the stable suspersion emulsion that can flow, be prone to measurement volumes, lets slip in the journey in storage layering or deposition to occur, handles and shakes and can restore to the original state, not caking.Topple over the back residue less than 10%, the residual excess in washing back is less than 1.0%; Lasting foaming characteristic (behind the 1min) is less than 10ml.
Embodiment one: chlopyrifos and the indoor virulence test (this test by Zhejiang Provincial Chemical Engineering Research Inst undertaken) of the different proportionings of spiral shell worm ethyl ester to scale insect:
Test the former medicine of used chlopyrifos by Zhejiang Xinnong Chemical Co.,Ltd provide, the former medicine of spiral shell worm ethyl ester provides by Bayer Cropscience (China) Co., Ltd; Spiral shell worm ethyl ester: the chlorpyrifos mixture proportioning is 1: 1,1: 3,1: 6,1: 9 and 1: the 12 o'clock indoor biologically active to scale insect, and the contrast medicament is spiral shell worm ethyl ester and chlopyrifos.The infusion process that test method adopts FAO to recommend, checkout facility result behind the 72h.According to co-toxicity coefficient (Co-Toxicity coefficient) computational methods of introductions such as Sun Yunpei, calculate the co-toxicity coefficient of mixture; With co-toxicity coefficient＞120 is synergistic effect, and 80～120 is summation action, and＜80 is antagonism, confirms whether synergy of mixture.Result of the test is seen table 1, table 2:
Table 1 chlopyrifos and indoor virulence and the co-toxicity coefficient (72h) of the different proportionings of spiral shell worm ethyl ester to scale insect
The different proportionings with chlopyrifos of table 2 spiral shell worm ethyl ester are to coccid toxicity index and co-toxicity coefficient analysis result
Test result shows: spiral shell worm ethyl ester and chlopyrifos to coccid 1: 1-1: showed as summation action at 6 o'clock; 1: 9-1: 12 show synergistic effect.The highest with spiral shell worm ethyl ester and chlopyrifos with 1: 9 virulence and co-toxicity coefficient, be best proportioning.
Embodiment two:
Table 3 spiral shell worm ethyl ester+chlopyrifos control oranges and tangerines coccid result of the tests (Kaihua County, Quzhou City plant protection unit)
Embodiment three:
Table 4 spiral shell worm ethyl ester+chlopyrifos control tomato Bemisia tabaci result of the test (Zhejiang A & F University)
More than two result of the tests show: test shows that spiral shell worm ethyl ester and chlopyrifos are mixed and can significantly improve chlopyrifos and spiral shell worm ethyl ester quick-acting and the control efficiency to citrus scale insect and tomato Bemisia tabaci; Especially (spiral shell worm ethyl ester: chlopyrifos=4: 36) 1000 times of liquid control efficiency are the most desirable, are the good prescriptions that is worth exploitation with 40% spiral shell worm ethyl ester chlopyrifos SE.
Claims (11)
1. compound insecticidal suspension emulsion that contains chlopyrifos and spiral shell worm ethyl ester is characterized in that containing by weight percentage following component:
Chlopyrifos 10-40%
Spiral shell worm ethyl ester 2-30%
Organic solvent 5-20%
Water surplus.
2. the compound insecticidal suspension emulsion that contains chlopyrifos and spiral shell worm ethyl ester as claimed in claim 1 is characterized in that also containing by weight percentage following component:
Emulsifier 5-12%
Cosurfactant 0-5%
Dispersant 2-6%
Wetting agent 1-3%
Antifreezing agent 0-5%
Thickener 0-3%
Antifoaming agent 0-0.4%.
3. according to claim 1 or claim 2 the compound insecticidal suspension emulsion that contains chlopyrifos and spiral shell worm ethyl ester is characterized in that the content sum of said by weight percentage chlopyrifos, spiral shell worm ethyl ester and organic solvent is not more than 65%.
4. the compound insecticidal suspension emulsion that contains chlopyrifos and spiral shell worm ethyl ester as claimed in claim 3 is characterized in that containing by weight percentage following component:
Chlopyrifos 20-30%
Spiral shell worm ethyl ester 5-20%
Organic solvent 5-10%
Emulsifier 5-10%
Cosurfactant 2-4%
Dispersant 2-4%
Wetting agent 1-2%
Antifreezing agent 2-5%
Thickener 2-3%
Antifoaming agent 0.2-0.4%
Water surplus.
5. the compound insecticidal suspension emulsion that contains chlopyrifos and spiral shell worm ethyl ester according to claim 4 is characterized in that:
Said organic solvent is selected from cyclohexanone, xylol, No. 1500 solvents, No. 1800 solvents, No. 2000 solvents, amylalcohol, isooctane or its mixtures;
Described emulsifier is selected from polyoxyethylene nonylphenol ether; APES; Fat alcohol ethoxyl compound; Styryl phenyl APEO; Alkyl phenol formaldehyde resin polyoxyethylene ether; Styrene phenol formaldehyde resin APEO; The polyoxyethylene polyoxypropylene block co-polyether; The secondary octyl phenol polyethenoxy ether; Castor oil polyoxyethylene ether; Fat alcohol alkoxy compound; Tallow ethyoxyl amine salt; Starch Sodium Octenyl Succinate; Polyoxyethylene ether phosphate salt; Alkyl phosphate salt; Naphthalene sulfonate salt or its mixture;
Said cosurfactant is selected from n-butanol, isobutanol, n-octyl alcohol or its mixture;
Described wetting agent is selected from EO/PO block polyether, AEO, fat alcohol ethoxyl compound, tallow ethyoxyl ammonium salt, alkylnaphthalene sulfonate, fatty alcohol polyoxyethylene ether sulfate, acyl group glutamate.Said dispersant is selected from naphthalene sulfonic acid condensate sodium salt, phenolsulfonic acid condensation product sodium salt, methyl naphthalene sulfonate formaldehyde condensate, sodium lignin sulfonate, sodium metnylene bis-naphthalene sulfonate, acrylate homopolymer sodium salt, polymeric polycarboxylic acid salt, dioctyl sodium sulphosuccinate salt, maleic acid-acrylic acid copolymer sodium salt or its mixture;
Said antifreezing agent is selected from ethylene glycol, PEG400, propane diols, glycerine, isopropyl alcohol or its mixture;
Described thickener is selected from xanthans, Magnesiumaluminumsilicate, sodium carboxymethylcellulose, organobentonite or its mixture;
Said antifoaming agent is silicone defoaming agent, polyether antifoam agent or its mixture;
Described water is deionized water or distilled water.
6. preparation method who contains the compound insecticidal suspension emulsion of chlopyrifos and spiral shell worm ethyl ester is characterized in that comprising following processing step:
A. the weight ratio according to spiral shell worm ethyl ester 2-30%, chlopyrifos 10-40%, organic solvent 5-20%, water surplus takes by weighing raw material;
B. with above-mentioned raw materials mixing, sand milling, filtration;
C. filtrate gets the suspension emulsion finished product through the high speed shear homogeneous.
7. preparation method as claimed in claim 6 is characterized in that the raw material that takes by weighing with weight ratio also comprises emulsifier 5-12%, dispersant 2-6%, wetting agent 1-3%, cosurfactant 0-5%, antifreezing agent 0-5%, thickener 0-3%, antifoaming agent 0-0.4%.
8. preparation method who contains the compound insecticidal suspension emulsion of chlopyrifos and spiral shell worm ethyl ester is characterized in that comprising following processing step:
A. the weight ratio according to spiral shell worm ethyl ester 2-30%, chlopyrifos 10-40%, organic solvent 5-20%, water surplus takes by weighing raw material respectively;
B. the spiral shell worm ethyl ester, the water that are taken by weighing are mixed sand milling, cross and to filter spiral shell worm ethyl ester suspending agent;
C. the chlopyrifos that is taken by weighing, organic solvent are mixed, be added under the high speed shear in the spiral shell worm ethyl ester suspending agent, high speed shear, mistake filter the suspension emulsion finished product.
9. preparation method as claimed in claim 8 is characterized in that the raw material that takes by weighing with weight ratio also comprises emulsifier 5-12%, dispersant 2-6%, wetting agent 1-3%, cosurfactant 0-5%, antifreezing agent 0-5%, thickener 0-3%, antifoaming agent 0-0.4%.
10. preparation method who contains the compound insecticidal suspension emulsion of chlopyrifos and spiral shell worm ethyl ester is characterized in that comprising following processing step:
A. the weight ratio according to spiral shell worm ethyl ester 2-30%, chlopyrifos 10-40%, organic solvent 5-20%, water surplus takes by weighing raw material respectively;
B. spiral shell worm ethyl ester is processed suspending agent;
C. chlopyrifos is processed aqueous emulsion
D. with above gained suspending agent and aqueous emulsion high speed shear, emulsifying, mistake filter suspension emulsion.
11. preparation method as claimed in claim 10 is characterized in that the raw material that takes by weighing with weight ratio also comprises emulsifier 5-12%, dispersant 2-6%, wetting agent 1-3%, cosurfactant 0-5%, antifreezing agent 0-5%, thickener 0-3%, antifoaming agent 0-0.4%.
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| CN107950565A (en) * | 2017-12-18 | 2018-04-24 | 青岛农业大学 | A kind of new pesticide combination |
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