CN102475092B - 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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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 compound insecticidal suspension emulsion and the preparation method of a kind of containing chlopyrifos and spiral shell worm ethyl ester.
Background technology:
Chlopyrifos (chlorpyrifos) is the broad spectrum insecticide of anticholinesterase, there is good tagging and stomach poison function, and there is certain stifling property, there is no interior suction and osmosis, the larva of the scale insect of firm hatching, aphid, mealybug, wood louse is had to good control efficiency, undesirable to forming the scale insect effect of wax coat, insect is 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 two-way interior suction conductive performance, and insecticidal spectrum is wide, and the lasting period is long.It is that fatty biosynthesis by interference insect causes larva dead, and insect is subject to medicine plant to death generally to need 3-5 days taking food.Due to its unique mechanism of action, can effectively prevent and treat the insect that existing insecticide is produced to resistance, as the sucking pest on citrus, apple, pears, vegetable crop: scale insect, aphid, mealybug, wood louse, trialeurodes vaporariorum, thrips etc.
Although spiral shell worm ethyl ester is effective, but quick-acting is slow, and peasant sees just medication after insect, thereby be later than administration time 7-10 days, and now a large amount of larva has been fixed on the growth site of plant, be subject to medicine plant to death generally also to need 3-5 days taking food, as being now mixed with a kind of medicament of quick-acting, using and just can kill off the insect pests rapidly, alleviate harm.Chlopyrifos is exactly ideal mixed medicament.
In actual production, chlopyrifos single dose was used and is prevented and treated for citrus, apple, vegetables, cotton-plant pest-insects with mixing of spiral shell worm ethyl ester single dose.But in actual use, encounter following several problem: 1, user can not determine the best proportioning of two medicines when bucket is mixed, thereby cannot obtain best preventive effect, and the expenses for prevention and control that increment use produces is high or unreasonable adapted makes control not cheap; 2, different brand chlopyrifos single doses has different quality (nearly more than 350 of the chlorpyrifos ec single doses of selling in China), and this can not be guaranteed the mixed quality of bucket, thereby control efficiency cannot be guaranteed.
So in the urgent need to researching and developing the complex preparation of a kind of spiral shell worm ethyl ester and chlopyrifos, to overcome the above problems.By biologicall test, screen and obtain rational composite proportioning, make the biological effect synergy between spiral shell worm ethyl ester and chlopyrifos reach best, both reached the effect of synergy, can reduce again the usage amount of medicament, alleviate the pressure to environment.The built agent of spiral shell worm ethyl ester and chlopyrifos is carried out to form formula research simultaneously, to ensure that the biologically active of two effective ingredients gives full play to, 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 compound insecticidal suspension emulsion of a kind of containing chlopyrifos and spiral shell worm ethyl ester and preparation method thereof is provided, and to solve the composite problem of chlopyrifos and spiral shell worm ethyl ester, for producing qualified composite product industrialization, provides technical support.
Above-mentioned purpose of the present invention is to realize by following technological means.
The compound insecticidal suspension emulsion of a kind of containing chlopyrifos provided by the present invention and spiral shell worm ethyl ester, contains following component by weight percentage:
Chlopyrifos 10-40%
Spiral shell worm ethyl ester 2-30%
Organic solvent 5-20%
Water surplus.
Also contain 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%
Defoamer 0-0.4%.
The content sum of described chlopyrifos, spiral shell worm ethyl ester and organic solvent is not more than 65% by weight percentage.
The compound insecticidal suspension emulsion of described containing chlopyrifos and spiral shell worm ethyl ester, preferably contains 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%
Defoamer 0.2-0.4%
Water surplus.
Described organic solvent is selected from cyclohexanone, dimethylbenzene, No. 1500 solvents, No. 1800 solvents, No. 2000 solvents, amylalcohol, isooctane or its mixtures;
Described emulsifier is selected from polyoxyethylene nonylphenol ether, alkylphenol polyoxyethylene, fat alcohol ethoxyl compound, styryl phenyl APEO, alkyl phenol formaldehyde resin polyoxyethylene ether, styrene phenol formaldehyde resin APEO, polyoxyethylene polyoxypropylene block co-polyether, 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,
Described cosurfactant is selected from n-butanol, isobutanol, n-octyl alcohol or its mixture;
Described wetting agent is selected from EO/PO block polyether, fatty alcohol-polyoxyethylene ether, fat alcohol ethoxyl compound, tallow ethyoxyl ammonium salt, alkylnaphthalene sulfonate, fatty alcohol polyoxyethylene ether sulfate, acyl group glutamate.Described 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;
Described 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;
Described defoamer is silicone defoaming agent, polyether antifoam agent or its mixture;
Described water is deionized water or distilled water.
The present invention also provides the preparation method of the compound insecticidal suspension emulsion of a kind of containing chlopyrifos and spiral shell worm ethyl ester, and it comprises following processing step:
A. according to the weight ratio of spiral shell worm ethyl ester 2-30%, chlopyrifos 10-40%, organic solvent 5-20%, water surplus, take raw material;
B. by above-mentioned raw materials mixing, sand milling, filtration;
C. filtrate obtains suspension emulsion finished product through high speed shear homogeneous.
The raw material that described preparation method takes 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%, defoamer 0-0.4%.
The present invention provides again the preparation method of the compound insecticidal suspension emulsion of a kind of containing chlopyrifos and spiral shell worm ethyl ester, and it comprises following processing step:
A. according to the weight ratio of spiral shell worm ethyl ester 2-30%, chlopyrifos 10-40%, organic solvent 5-20%, water surplus, take respectively raw material;
B. taken spiral shell worm ethyl ester, water mixed to sand milling, filter to obtain spiral shell worm ethyl ester suspending agent;
C. taken chlopyrifos, organic solvent are mixed, under high speed shear, be added in spiral shell worm ethyl ester suspending agent, high speed shear, filter to obtain suspension emulsion finished product.
The raw material that described preparation method takes 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%, defoamer 0-0.4%.
The present invention provides the preparation method of the compound insecticidal suspension emulsion of a kind of containing chlopyrifos and spiral shell worm ethyl ester again, and it comprises following processing step:
A. according to the weight ratio of spiral shell worm ethyl ester 2-30%, chlopyrifos 10-40%, organic solvent 5-20%, water surplus, take respectively raw material;
B. spiral shell worm ethyl ester is made to suspending agent;
C. chlopyrifos is made to aqueous emulsion;
D. by above gained suspending agent and aqueous emulsion high speed shear, emulsifying, filter to obtain suspension emulsion.
The raw material that described preparation method takes 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%, defoamer 0-0.4%.
Compound insecticidal suspension emulsion containing 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 spiral shell worm ethyl ester, solve insect to the pesticide resistance of chlopyrifos and lasting period problem, reduce the higher problem of spiral shell worm ethyl ester cost of using separately simultaneously.
Containing chlopyrifos provided by the present invention and spiral shell worm ethyl ester compound insecticidal suspension emulsion outward appearance homogeneous; Easy mobility; Stability of emulsion is qualified; Cold and hot material storage reason qualified stability; Under the condition of 54 ± 1 ℃, heat storage is two weeks, and chlopyrifos and spiral shell worm ethyl ester resolution ratio are all less than 5%, and after storage, preparation stability of emulsion is qualified.
There is following technology of preparing difficult point in the compound insecticidal suspension emulsion of containing chlopyrifos and spiral shell worm ethyl ester and preparation thereof: 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 Field, the oil droplet of suspension and solid particle can sink gradually, and in addition because there is model ylid bloom action power between oil droplet and solid particle, easily attracting each other agglomeration occurs and further accelerates sedimentation, produces and piles up.Pile up when lighter, it is denseer thick that preparation outward appearance is bottom, up weakens gradually; While crossing closs packing, there is flocculation, even produce precipitation or breakdown of emulsion (analysing oil) phenomenon, cause and cannot again disperse to form homogeneous system.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 solves technological difficulties prepared by aforementioned suspension emulsion by following approach:
1. adopt the surfactant that has stronger adsorption capacity on agricultural chemicals oil droplet surface, as polyoxyethylene polyoxypropylene block co-polyether etc., on oil droplet surface, form more stable sterically hindered effect, prevent coalescent;
2. select suitable surfactant to carry out composite, make composite emulsifier form the higher compound interface film of mechanical strength on agricultural chemicals oil droplet surface, interfacial film intensity is higher, is difficult for occurring coalescent increase when oil droplet collides mutually, and system is just more stable;
3. select suitable anion auxiliary agent, as tallow ethyoxyl amine salt, phosphates, naphthalene sulfonate salt etc., strengthen Zeta potential gesture, make between oil droplet, electrostatic repulsion forces strengthens between solid particle, is difficult for occurring coalescent;
4. select suitable process route and technological parameter, make the particle size distribution range of oil droplet and particle narrower, meso-position radius is less, slow down settling velocity, and significantly alleviate Ostwald ripening phenomenon;
5. keeping in the good mobility of preparation and dispersed situation, utilize the 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, prevent generation precipitation or the demulsifying phenomenon of shelf life in the phase;
Through a large amount of tests, we have selected chlopyrifos and spiral shell worm ethyl ester to be developed to suspension emulsion.In suspension emulsion, at least containing two kinds of water-fast active ingredients, with solia particle and fine liquid pearl form, be stably dispersed in and take in the heterogeneous liquid that water is continuous phase, have advantages of suspending agent and aqueous emulsion, is a kind of Water-borne modification green pesticide form.On stream; we have overcome suspension emulsion under Action of Gravity Field; the oil droplet and the solid particle that suspend can sink gradually; and between oil droplet and solid particle under van der Waals interaction; and produce agglomeration, even generation precipitation or breakdown of emulsion (analysing oil) phenomenon, cause the key technology difficult point that cannot again disperse to form homogeneous system.Said preparation is waterborne preparation, in production process, without dust, in use procedure, without imbedibility health risk, can make the preparation of high-load simultaneously, for producing, promoting the use of, provides possibility.
This case, by a large amount of raw both appropriate proportionings of experiment sieving of surveying, reaches the insurmountable problem of single dose that solution is encountered in producing cost-effectively; Again by pharmaceutical formulation screen, production technology develops, the product that formation can industrialization.
Through test of many times, when the content sum of described chlopyrifos, spiral shell worm ethyl ester and organic solvent is greater than 65% by weight percentage, because of institute's water content in preparation very few, too dense thick dispersiveness and the pourability of causing of the product of preparing is not good, unfavorable production and use, also can be because the multipair environment of the remaining mistake of Packaging Bottle Chinese medicine produces unnecessary pollution, in formula, very few also can causing of the water yield cannot make qualified formulation products simultaneously.
Provided by the present invention have following characteristics containing spiral shell worm ethyl ester chlorpyrifos mixture desinsection suspension emulsion under real use:
1, found desirable cosolvent, emulsifier, dispersant, wetting agent and rational production method, made spiral shell worm ethyl ester can form suspending agent system, and can make chlopyrifos can stably exist with the form of small oil droplet in this system.
2, quick-acting is obviously better than spiral shell worm ethyl ester single dose, has retained again long advantage of spiral shell worm ethyl ester single dose drug effect phase simultaneously; Insecticidal spectrum is extensively in spiral shell worm ethyl ester single dose and chlopyrifos single dose, and medicament is also significantly improved.
3,, due to reasonable mixture ratio, when drug effect promotes, reduced cost accounting, and alleviated the impact on environment.
4, water, as primary solvent, reduces environmental pollution, and conservation cost can be avoided the impact of international petroleum market price again simultaneously.
5, solvent-free smell, to eye nonirritant, to people's dermal toxicity significantly lower than missible oil.
6, manufacture and while using safety and processing cost low.
Embodiment:
In order better to understand essence of an invention, below just better utilize example to describe the technology contents of invention in detail.But content of the present invention is not only confined to this, the inseparable change of essence all and of the present invention and scope, modification, distortion or other are used and apply, within being all regarded as falling into scope of the present invention.
In 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, dimethylbenzene, No. 1500 solvents (Jiaxing City Zhong He petrochemical industry Co., Ltd), No. 1800 solvents (Huzhou Bohai petroleum Chemical Co., Ltd.), No. 2000 solvents (large 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 to abundant mixing, put into again high shear homogenized milk agent high speed and shear corase grind and homogeneous, pump is to sand milling in sand mill again, sand milling, to certain particle diameter, obtains suspending agent after refiltering.In suspending agent, contain 20.0% spiral shell worm ethyl ester, D
90particle diameter is 3-5 micron.Again 10% 20.0% spiral shell worm ethyl ester suspending agent, chlopyrifos 40.0%, dimethylbenzene 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 to abundant mixing, high speed shear, emulsifying, filtration make suspension emulsion, and suspension emulsion is containing 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 again high shear homogenized milk agent high speed and shear corase grind and homogeneous, pump is to sand milling in sand mill again, sand milling, to certain particle diameter, obtains suspending agent after refiltering.In suspending agent, contain 25.0% spiral shell worm ethyl ester, D
90particle diameter is 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 make suspension emulsion, and suspension emulsion is containing 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%, fatty alcohol-polyoxyethylene ether 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 again high shear homogenized milk agent high speed and shear corase grind and homogeneous, pump is to sand milling in sand mill again, sand milling, to certain particle diameter, obtains suspending agent after refiltering.In suspending agent, contain 40% spiral shell worm ethyl ester, D
90particle diameter is 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%, alkylphenol polyoxyethylene 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 make suspension emulsion, and suspension emulsion is containing the reactive compound of 30% content.
Embodiment 4:
30% reactive compound (20.0% spiral shell worm ethyl ester and 10.0% chlopyrifos composition): by 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 water supply be fully uniformly mixed rear sand milling to meso-position radius in 1-5 micron, filter main, through high speed shear homogeneous, make suspension emulsion again, suspension emulsion is containing the reactive compound of 30% content.
Embodiment 5:
35% reactive compound (5.0% spiral shell worm ethyl ester and 30.0% chlopyrifos composition): by 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 is supplied abundant mixing, put into again high shear homogenized milk agent high speed and shear corase grind and homogeneous, pump is to sand milling in sand mill again, sand milling is to certain particle diameter, after refiltering, obtain suspending agent, in suspending agent, contain 20.0.% spiral shell worm ethyl ester, D
90particle diameter is 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 to abundant mixing, high speed shear, emulsifying, filtration make suspension emulsion, and suspension emulsion is containing the reactive compound of 35% content.
Embodiment 6:
40% reactive compound (30.0% spiral shell worm ethyl ester and 10.0% chlopyrifos composition): by spiral shell worm ethyl ester 30.0%, chlopyrifos 10.0%, fatty alcohol-polyoxyethylene ether 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 water is supplied abundant mixing, put into again high shear homogenized milk agent high speed and shear corase grind and homogeneous, pump is to sand milling in sand mill again, sand milling is to certain particle diameter, after refiltering, obtain suspension emulsion, suspension emulsion is containing 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 supplied and be fully uniformly mixed afterwards, put into again sand milling in sand mill, until meso-position radius in 1-5 micron, filters and obtains 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 to abundant mixing, after high speed shear emulsifying, make 25% chlorpyrifos aqueous emulsion; Again 20% 25.0% spiral shell worm ethyl ester suspending agent, 80% 25% chlorpyrifos aqueous emulsion are fully uniformly mixed, and through high speed shear homogeneous, make the reactive compound containing 25% content.
Above sample be can flow, the easy stable suspersion emulsion of measurement volumes, in storage, let slip in journey and may occur layering or precipitation, handle and shake and can restore to the original state, not caking.Topple over rear residue and be less than 10%, after washing, residual excess is less than 1.0%; Lasting foaming characteristic (after 1min) is less than 10ml.
Embodiment mono-: chlopyrifos and the different proportionings of spiral shell worm ethyl ester are to the indoor virulence test of scale insect (this test is undertaken by Zhejiang Provincial Chemical Engineering Research Inst):
Test that chlopyrifos Yuan Yaoyou used Zhejiang Xinnong Chemical Co.,Ltd provides, the former medicine of spiral shell worm ethyl ester is provided by Bayer Cropscience (China) Co., Ltd; Spiral shell worm ethyl ester: chlorpyrifos mixture proportioning is 1: 1,1: 3,1: 6,1: 9 and 1: the 12 o'clock indoor biologically active to scale insect, contrast medicament is spiral shell worm ethyl ester and chlopyrifos.The infusion process that test method adopts FAO to recommend, checkout facility result after 72h.According to co-toxicity coefficient (Co-Toxicity coefficient) computational methods of the introductions such as Sun Yunpei, calculate the co-toxicity coefficient of mixture; Take co-toxicity coefficient > 120 as synergistic effect, and 80～120 is summation action, and < 80 is antagonism, determines whether synergy of mixture.Result of the test in Table 1, table 2:
Table 1 chlopyrifos from the different proportionings of spiral shell worm ethyl ester to the indoor virulence of scale insect and co-toxicity coefficient (72h)
Table 2 spiral shell worm ethyl ester proportionings different from chlopyrifos 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: show as summation action at 6 o'clock; 1: 9-1: 12 show synergistic effect.The highest with virulence and the co-toxicity coefficient of 1: 9 with spiral shell worm ethyl ester and chlopyrifos, be best proportioning.
Embodiment bis-:
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 tri-:
Table 4 spiral shell worm ethyl ester+chlopyrifos control tomato Bemisia tabaci result of the test (Zhejiang A & F University)
Above two result of the tests show: test shows that spiral shell worm ethyl ester and chlopyrifos are mixed and can significantly improve chlopyrifos and quick-acting and the control efficiency of spiral shell worm ethyl ester to citrus scale insect and tomato Bemisia tabaci, especially with 40% spiral shell worm ethyl ester chlopyrifos SE, (spiral shell worm ethyl ester: chlopyrifos=4: 36) 1000 times of liquid control efficiency are the most desirable is the good formula that is worth exploitation.
Claims (1)
1. a compound insecticidal suspension emulsion for containing chlopyrifos and spiral shell worm ethyl ester, is characterized in that containing by weight percentage following component:
Described organic solvent is selected from cyclohexanone, dimethylbenzene, No. 1500 solvents, No. 1800 solvents, No. 2000 solvents, amylalcohol, isooctane or its mixtures;
Described emulsifier is selected from polyoxyethylene nonylphenol ether, fat alcohol ethoxyl compound, styryl phenyl APEO, alkyl phenol formaldehyde resin polyoxyethylene ether, styrene phenol formaldehyde resin APEO, polyoxyethylene polyoxypropylene block co-polyether, secondary octyl phenol polyethenoxy ether, castor oil polyoxyethylene ether, starch Sodium Octenyl Succinate, polyoxyethylene ether phosphate salt, alkyl phosphate salt, naphthalene sulfonate salt or its mixture;
Described cosurfactant is selected from n-butanol, isobutanol, n-octyl alcohol or its mixture;
Described wetting agent is selected from EO/PO block polyether, fat alcohol ethoxyl compound, alkylnaphthalene sulfonate, fatty alcohol polyoxyethylene ether sulfate, acyl group glutamate;
Described 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;
Described 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;
Described defoamer is silicone defoaming agent, polyether antifoam agent or its mixture;
Described water is deionized water or distilled water.
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| CN103283774B (en) * | 2012-02-22 | 2016-02-17 | 陕西美邦农药有限公司 | A kind of Pesticidal combination containing spiral shell worm ethyl ester |
| CN102726450B (en) * | 2012-07-23 | 2014-10-22 | 中国农业大学 | Pesticide suspension emulsion containing spirotetramat as well as preparation method and application thereof |
| CN103120178B (en) * | 2013-02-07 | 2015-09-09 | 南京红太阳股份有限公司 | A kind of water baseization chlopyrifos novel form ZW and processing thereof and application |
| CN104286018A (en) * | 2014-09-18 | 2015-01-21 | 青岛润鑫伟业科贸有限公司 | Efficient insecticide containing chlorpyrifos, triazophos and spirotetramat |
| CN106165692A (en) * | 2016-07-22 | 2016-11-30 | 深圳诺普信农化股份有限公司 | Compound insecticidal liquid preparation containing spiral shell worm ethyl ester |
| CN107950565B (en) * | 2017-12-18 | 2021-06-29 | 青岛农业大学 | Pesticide composition |
| WO2024003905A1 (en) * | 2022-06-30 | 2024-01-04 | Adama Makhteshim Ltd. | Insecticide formulations with built-in adjuvants |
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