CN101305717B - Insecticidal spray EC and its preparation method - Google Patents
Insecticidal spray EC and its preparation method Download PDFInfo
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- CN101305717B CN101305717B CN2008100635470A CN200810063547A CN101305717B CN 101305717 B CN101305717 B CN 101305717B CN 2008100635470 A CN2008100635470 A CN 2008100635470A CN 200810063547 A CN200810063547 A CN 200810063547A CN 101305717 B CN101305717 B CN 101305717B
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Abstract
The invention relates to a disinsection sprinkling oil concentrate, which mainly composed of components with the following mass content: 40 to 65 percent of liquid paraffin, 2 to 5 percent of jinggangmycin, 1 to 3 percent of avermectin, 2 to 10 percent of tea saponin, 0.5 to 2 percent of water soluble extractive of plocamium telfairiae harv, 0.5 to 6 percent of water soluble extractive of tobacco leaves, 1.5 to 3 percent of emulsifier and the balancing amount of water; the emulsifier is mixture of sapn and tween with the mass ratio of 3: 1. The disinsection sprinkling oil concentrate of the invention has broad spectrum bacteriostasis and sterilization effect, quick action and long action are combined together, an efficacy period of 35 days can be maintained, no toxicity can be left on human and livestock, the environment can not be polluted, the effective drug consumption can be reduced, the generation of drug fastness can be suspended, and thereby the disinsection sprinkling oil concentrate can be used for the disinsection and the prophylaxis to fruits, vegetables, garden flowers, lawns, and urban gardens and trees.
Description
(1) technical field
The present invention relates to insecticidal spray EC of a kind of safety and environmental protection and preparation method thereof.
(2) background technology
At present most agricultural chemicals are chemical pesticides, have higher even high toxicity, and in the process of spraying and afterwards residual of agricultural chemicals is to environment and humanly produced serious harmful effect; Chemical pesticide makes insect produce tangible pesticide resistance simultaneously, causes dispenser dosage to continue to increase, and control efficiency worse and worse.Therefore, press for a kind of insecticide, substitute highly toxic chemical pesticide with broad spectrum disinfestation effect, safety and environmental protection.
(3) summary of the invention
The object of the invention provides a kind of insecticidal spray EC with broad spectrum disinfestation effect, safety and environmental protection and preparation method thereof.
The technical solution used in the present invention is:
A kind of insecticidal spray EC mainly is made into by the following component of mass content:
Atoleine 40～65%
Jinggangmycin 2～5%
Avermectin 1～3%
Tea Saponin 2～10%
The water-soluble extract 0.5～2% of a sea red algae
The water-soluble extract 0.5～6% of tobacco leaf
Emulsifier (food-grade) 1.5～3%
Surplus is a water; Described emulsifier is sapn and 3: 1 mixture of tween mass ratio.
Said components is the active principle of insecticidal spray EC, and each constituent mass percentage composition is the percentage of each ingredients constitute said components sum, does not comprise regulating the used glacial acetic acid of pH value.
Employed mineral oil is the mixture through refining one or more, requirement reaches the food-grade requirement, and its degree of saturation is more than 99%, wherein paraffin hydrocarbon content is 60～90% (being preferably 69～90%), naphthene content is in 40～10% (best 31～10%), and aromatic hydrocarbon content approaches zero; Carbon atom be distributed in 15～35, be preferably 20～30; And require the good security of ultraviolet light.
Tea Saponin belongs to pentacyclic triterpene saponin (C
57H
90O
26), so have another name called the tea saponin, by a class candy glucoside compound that extracts in the tea tree seed, it is a kind of good natural surfactant, not only has good emulsifying, foaming, disperse, infiltration, wetting isoreactivity effect, with the Tea Saponin is that the refining environmental protection type agricultural chemical auxiliary agent that forms of main body can be widely used in the purpose that insecticide, bactericide, weed killer herbicide etc. reach synergy, solubilising, attenuation, simultaneously because the repellent and the bio-hormone effect of Tea Saponin itself also are a kind of good biopesticides, and can also the stimulating organism growth.As the wetting agent of wettable agricultural chemicals, can not only obviously improve the wet performance of agricultural chemicals, and can effectively improve the suspensibility of agricultural chemicals; More as its superiority of water aqua type insecticides adjuvant, it does not contain the metal ion that diminishes pesticide quality, because of the neutral meta-acid of its pH value, helps the storage of agricultural chemicals; As missible oil type agricultural chemicals, its good plate-out ability, permeability and emulsifying dispersivity are a kind of new and effective insecticides adjuvants, because the surface-active effect of Tea Saponin can make the synergistic effect of agricultural chemicals minimizing consumption obvious.
The technical indicator of above-mentioned Tea Saponin: outward appearance is light yellow powder, and active matter content 〉=50%, foaming power are 160～190 millimeters, surface tension: 47～51 milli ox/rice.
Tea Saponin also is a kind of slow-acting type insecticide, it has haemocylolysis, enter interior its protoplasm that destroys of pest body and cause insect death, it has very strong surface-active and diffusivity simultaneously, be homogeneous film at the insect body surface, the insect that tags has very strong moisture absorption again, after absorbing dew insect is soaked in soup, its strong adhesion more helps the drug effect performance.Soil insect is the insect that is difficult to control, is the special-purpose insecticide of host development with the Tea Saponin, not only can kill cutworm, earthworm, nematode etc. effectively, and can not cause soil pollution, helps environmental protection.The Tea Saponin concentration of using of splashing separately is 500～1200 times of dilutions.。
Avermectin (Abamectin) is the macrolides Biocidal miticide that produces by the biofermentation bacterial metabolism.Pure product are white crystal, and molecular formula is C
48H
72O
14, be dissolved in methyl alcohol, ethanol, acetone isopolarity organic solvent, be insoluble in non-polar solvens such as aliphatic hydrocarbon, water insoluble.Avermectin has desirable insect killing effect to insect common on the agricultural, mite such as two spotted spider mite, white spider, diamond-back moth, liriomyza bryoniae, pear sucker, trialeurodes vaporariorum etc., not having cross resistance with other insecticidal/acaricidal agent, is present important super-high-efficient Biocidal miticide kind.Having inherited the biological characteristics of Avermectin by the emamectin-benzoate of Avermectin transformation, insects such as beet armyworm are shown higher insecticidal activity, is the acaricidal ideal substitute kind of abamectin pest killing.But Avermectin exists, and toxicity height, quick-acting are poor, use cost height, most worm, mite be to problems such as it develop immunity to drugs, reduce toxicity and cost, overcome and delay therefore that pesticide resistance produces is present urgent problem.
The present invention preferably resolves the problems referred to above:
High and the cost height of toxicity: missible oil of the present invention has reduced using dosage when guaranteeing original insecticidal activity.
Quick-acting is poor: because of the characteristic of Avermectin is to be dissolved in methyl alcohol, ethanol, acetone isopolarity organic solvent, be insoluble in non-polar solvens such as aliphatic hydrocarbon, and water insoluble.Therefore spray with the aqua form in use and be difficult to active ingredient is acted on polypide.Therefore the present invention program helps the effect of active ingredient to polypide because the stifling quick-acting insecticidal actions of auxiliary nicotine owing to be in emulsification system, become water aqua type simultaneously during use.
Pesticide resistance: missible oil of the present invention and other insect disinfestation component be composite to have synergy, and its pesticide resistance will obviously descend.
Jinggangmycin is the antibiotic that a kind of actinomycetes produce, and is the kind of output and consumption maximum in China's antibiotic.Pure product are white powder, and molecular formula is C
20H
35O
13, soluble in water, inhale therapeutic action in having, stable in neutral and weak acid, weak base medium under the normal temperature.To people and animals' low toxicity, to fish, honeybee safety, the longevity of residure can reach 15～20 days, can use with various sterilization, insecticide.Jinggangmycin is used for preventing and treating the damping off of rice sheath blight disease, false smut and vegetable sprout term, white thin,tough silk etc. more; Mix use with other insecticide, have than independent use desinsection faster speed and better effect, not only can desinsection, also can prevent disease simultaneously, improved integrated control effect, reduced pest resistance to insecticide and production cost.
A sea red algae (Plocamium telfairiae Harv) is a Rhodophyta Gigartinales sea red section sea red genus marine alga, be grown on the low tide band rock or Shi Zhaozhong more, the southern and northern coastal distribution that all has of China, Halogen monoterpene, many halogen of ring-type monoterpene and contain oxygen halo monoterpene etc. in the frond, its extract has antibacterial activity, can be used as agricultural chemicals, maduca sexta, noctuid and mosquito larvae are all had inhibitory or killing effect, and its inhibitory or killing effect intensity surpasses the Padan (Padan) of nereistoxin.The contained red seaweed polysaccharide (a class galactan sulfate) of frond not only has significant antiviral activity, also is simultaneously the wall built-up adhesive of good emulsifier, stabilizing agent and spray crop, helps and reduces drop and prolong drug effect.
The water-soluble algae extract of a described sea red algae is that the water extract of a conventional sea red algae is water-soluble, among the present invention, a described sea red algae extract is water-soluble can be made by following method: (1) is got and is done a sea red algae, pulverize, 80～100 ℃ of extractings of water of 8～10 times of quality of adding 0.5～2 hour, centrifugal filtration gets extract I; (2) get a dried sea red algae in addition, the extract I that adds 8～10 times of quality, extracting is 24～36 hours under 90～100 ℃ of stirrings, centrifugal filtration gets extract II, extract II vacuum concentration to relative density is 1.05～1.15, the water-soluble extract of a described sea red algae (monoterpene mass content about 1.5%, total polysaccharides content about 2.7%).Step (2) gained filter residue can carry out the operation of step (1) once more, obtains the extracting that extract I is used further to a sea red algae in the step (2), and above-mentioned steps can repeat.
Be rich in nicotine (C in the tobacco
10H
14N
2), have another name called nicotine, be good active insecticidal components, its insecticidal mechanism is that paralysis is neural, the steam of nicotine can be in any part intrusive body of polypide and the performance toxic action.Because the volatile generation fumigation action of nicotine is a kind of fast-acting type insecticide.Can prevent and treat aphid, thrips, leaf roller, heart-eating worm, leaf miner, cabbage caterpillar, plant hopper and the leafhopper etc. of fruit tree, vegetables, tea and cotton etc.
The water-soluble extract of described tobacco leaf is the water extract of conventional tobacco leaf, among the present invention, the water-soluble extract of described tobacco leaf can be made by following method: (1) gets dry tobacco leaf, pulverizes, 70～80 ℃ of extractings of water 1～2 hour that add 8～10 times of quality, squeeze extract I; (2) get dry tobacco leaf in addition, add the extract I of 8～10 times of quality, extracting is 2～4 hours under 70～80 ℃ of stirrings, squeeze extract II, extract II vacuum concentration to relative density is 1.05～1.15, gets the water-soluble extract of described tobacco leaf (nicotine mass content about 1.2%).Step (2) gained filter residue can carry out the operation of step (1) once more, obtains the extracting that extract I is used further to tobacco leaf in the step (2), and above-mentioned steps can repeat.
Preferably, described sapn is a sorbester p38, and described tween is a Tween-60.Sorbester p38 (Span-65), promptly the anhydrous sorbitol tristearate is dissolved in organic solvents such as hot ethanol, toluene, is not used in water, can be scattered in the hot water, and HLB value 4.5 is the lipophile nonionic emulsifier, and safety non-toxic is non-stimulated; Tween-60 (Tween-60), i.e. polyoxyethylene sorbitol acid anhydride single-hard ester acid ester, water-soluble, ethanol, propyl alcohol equal solvent can be scattered in mineral oil, and mineral oil is had special emulsibility, belong to the hydrophily nonionic emulsifier, HLB value 15.3.
The invention still further relates to the method for the described insecticidal spray EC of preparation, the main raw materials in proportion for preparing described insecticidal spray EC is: atoleine 40～65%, jinggangmycin 2～5%, Avermectin 1～3%, the water-soluble extract 0.5～2% of Tea Saponin 2～10% a sea red algae, the water-soluble extract 0.5～6% of tobacco leaf, emulsifier 1.5～3%, surplus is a water; Described emulsifier is sapn and 3: 1 mixture of tween mass ratio; Described method comprises:
(1) jinggangmycin of getting formula ratio is dissolved in the water of formula ratio 1/3～2/3, obtains the jinggangmycin aqueous solution; The Avermectin of getting formula ratio is dissolved in the water of formula ratio 1/3～2/3, obtains the Avermectin aqueous solution; The sapn of formula ratio is dissolved in the atoleine of formula ratio, and is stand-by;
(2) add the water-soluble extract of tobacco leaf, the water-soluble extract of a sea red algae, the jinggangmycin aqueous solution and the Avermectin aqueous solution in the reactor, in high speed shear, add Tea Saponin, mixing also is warming up to 70～80 ℃, adds the tween of formula ratio, the high speed shear dispersion and emulsion;
(3) in reactor, add the atoleine that is dissolved with sapn that 1/3 step of measuring (1) obtains, high speed shear 10～15 minutes; Add the atoleine that is dissolved with sapn that 2/3 step of measuring (1) obtains again, high speed shear 25～30 minutes, it is 4.5 that glacial acetic acid is regulated the pH value, 200kg/cm
2Homogeneous obtains described insecticidal spray EC.
Preferably, the main raw materials in proportion for preparing described insecticidal spray EC is: atoleine 50%, jinggangmycin 3%, Avermectin 2%, Tea Saponin 6%, the water-soluble extract 1% of a sea red algae, the water-soluble extract 4% of tobacco leaf, sorbester p38 1.5%, Tween-60 0.5%, water 32%; Described method is as follows:
(1) get a sea red algae, pulverize, 90 ℃ of extractings of water of 10 times of quality of adding 0.5 hour, centrifugal filtration gets extract I; Other gets a sea red algae, adds the extract I of 10 times of quality, and extracting is 30 hours under 90 ℃ of stirrings, and centrifugal filtration gets extract II, and extract II vacuum concentration to relative density is 1.05, gets the water-soluble extract of a described sea red algae, and is stand-by;
(2) get dry tobacco leaf, pulverize, add 75 ℃ of extractings of water 1 hour of 8 times of quality, squeeze extract I; Other gets dry tobacco leaf, adds the extract I of 8 times of quality, and extracting is 2 hours under 75 ℃ of stirrings, squeeze extract II, extract II vacuum concentration to relative density is 1.05, the water-soluble extract of described tobacco leaf, stand-by;
(3) jinggangmycin of getting formula ratio is dissolved in the water of formula ratio 1/2, obtains the jinggangmycin aqueous solution; The Avermectin of getting formula ratio is dissolved in the water of formula ratio 1/2, obtains the Avermectin aqueous solution; The sorbester p38 of formula ratio is dissolved in the atoleine of formula ratio, and is stand-by;
(4) add the water-soluble extract of tobacco leaf, the water-soluble extract of a sea red algae, the jinggangmycin aqueous solution and the Avermectin aqueous solution in the reactor, in high speed shear, add Tea Saponin, mixing also is warming up to 70～80 ℃, adds the Tween-60 of formula ratio, the high speed shear dispersion and emulsion;
(5) in reactor, add the atoleine that is dissolved with sapn that 1/3 step of measuring (1) obtains, high speed shear 10 minutes; Add the atoleine that is dissolved with sapn that 2/3 step of measuring (1) obtains again, high speed shear 30 minutes, regulating the pH value with glacial acetic acid is 4.5,200kg/cm
2Homogeneous obtains described insecticidal spray EC.
The present invention utilizes physical principle, the mixture of one or more special mineral oil is sprayed at uniformly blade face and/or the rhizome surface of crop, make the insect surface be covered with the fine droplet of mineral oil, the pore that stops up the insect surface by drop reaches the purpose that makes insect death by suffocation, can be applicable among agricultural, forestry, the gardening, not only hypotoxicity reaches food-grade, and insecticidal effect has broad spectrum activity, to natural enemies security, environmentally safe, duration of efficacy is long, and some disease is also had control efficiency, can use separately, also can use with other agriculture chemical compoundings.
When using separately, described insecticidal spray EC is converted the water dilution use, converting the water ratio is 1: 100～1: 500.Concrete using method: stir after the dilution and use, when big, in spray process, need to stir once more in order to avoid the profit layering as if crop area with atomizer spray; For Different Crop and insect pest, converting the water ratio can be different; During spraying, crop blade face, blade back, rhizome etc. should be sprayed to all moistening, but till the firm dropping liquid; Should not at high temperature spray during use, also should not use in the rainy day.
With the composite use of other chemical pesticides the time, converting the water ratio can be 1: 50～1: 1000, but needs significant care for some chemical pesticides that contain sulphur, phosphorus when being mixed, and to avoid poisoning.
Insecticidal spray EC of the present invention has wide spectrum and presses down effect extremely, quick-acting and long-acting combining, can keep 35 days drug effect phases, to people and animals' avirulence, environmentally safe, can reduce effective dosage and delay its pesticide resistance producing, can be used for the disinsection prophylaxis of fruits and vegetables, vegetables, horticulture and flower, meadow, city trees and shrubs trees etc.
(4) embodiment
The present invention is described further below in conjunction with specific embodiment, but protection scope of the present invention is not limited in this:
Embodiment 1: the spray EC preparation
The raw material proportioning:
Atoleine (PRIMOL352-high viscosity 70 types of Mobil mobil White Mineral Oil) 50%, jinggangmycin (Qianjiang Biochemistry Co., Ltd., Zhejiang Prov.) 3%, Avermectin (Hebei Weiyuan Biochemical Co., Ltd.) 2%, Tea Saponin (Changshan branch company of Zhejiang Orient Tea Development Co., Ltd.) 6%, the water-soluble extract 1% of a sea red algae, the water-soluble extract 4% of tobacco leaf, sorbester p38 (the clear and bright chemical industry in Wenzhou Co., Ltd) 1.5%, Tween-60 (the clear and bright chemical industry in Wenzhou Co., Ltd) 0.5%, water 32%;
Method step:
(1) get a sea red algae (Kunshan one great algae is Co., Ltd already) 10kg, pulverize, 90 ℃ of extractings of water of 10 times of quality of adding 0.5 hour, centrifugal filtration gets extract I; Other gets a sea red algae 8kg, adds the extract I of 10 times of quality, and extracting is 30 hours under 90 ℃ of stirrings, and centrifugal filtration gets extract II, and extract II vacuum concentration to relative density is 1.05, gets the water-soluble extract of a described sea red algae, and is stand-by;
(2) get dry tobacco leaf (it is peaceful to derive from Bijie Prefecture, Guizhou Province prestige), pulverize 10kg, add 75 ℃ of extractings of water 1 hour of 8 times of quality, squeeze extract I; Other gets dry tobacco leaf 8kg, adds the extract I of 8 times of quality, and extracting is 2 hours under 75 ℃ of stirrings, squeeze extract II, extract II vacuum concentration to relative density is 1.05, the water-soluble extract of described tobacco leaf, stand-by;
(3) jinggangmycin of getting formula ratio is dissolved in the water of formula ratio 1/2, obtains the jinggangmycin aqueous solution; The Avermectin of getting formula ratio is dissolved in the water of formula ratio 1/2, obtains the Avermectin aqueous solution; The sorbester p38 of formula ratio is dissolved in the atoleine of formula ratio, and is stand-by;
(4) add the water-soluble extract of tobacco leaf, the water-soluble extract of a sea red algae, the jinggangmycin aqueous solution and the Avermectin aqueous solution in the reactor, high speed shear 10 minutes, Tea Saponin adds in the high speed shear process, mixing also is warming up to 70～80 ℃, the Tween-60 that adds formula ratio, the high speed shear dispersion and emulsion;
(5) add the atoleine that is dissolved with sapn that 1/3 step of measuring (1) obtains in reactor, high speed shear became emulsion oil-in-water in 10 minutes; The atoleine that is dissolved with sapn that obtains of step (1) that adds 2/3 amount again, high speed shear after 30 minutes phase transformation become water-in-oil emulsion, be 4.5 with food-grade glacial acetic acid (commercially available) adjusting pH value, high pressure homogenizer 200kg/cm
2Homogeneous obtains described insecticidal spray EC.
Embodiment 2: the spray EC preparation
The raw material proportioning:
Atoleine 40%, jinggangmycin 5%, Avermectin 3%, Tea Saponin 8%, the water-soluble extract 1.5% of a sea red algae, the water-soluble extract 6% of tobacco leaf, sorbester p38 1.8%, Tween-60 0.6%, water 34.1%;
Method step:
(1) get a sea red algae 10kg, pulverize, 90 ℃ of extractings of water of 10 times of quality of adding 0.5 hour, centrifugal filtration gets extract I; Other gets a sea red algae 8kg, adds 10 times of extract I, and extracting is 30 hours under 90 ℃ of stirrings, and centrifugal filtration gets extract II, and extract II vacuum concentration to relative density is 1.01, gets the water-soluble extract of a described sea red algae, and is stand-by;
(2) get dry tobacco leaf 10kg, pulverize, add 75 ℃ of extractings of water 1 hour of 8 times of quality, squeeze extract I; Other gets dry tobacco leaf 8kg, adds the extract I of 8 times of quality, and extracting is 2 hours under 75 ℃ of stirrings, squeeze extract II, extract II vacuum concentration to relative density is 1.02, the water-soluble extract of described tobacco leaf, stand-by;
(3) jinggangmycin of getting formula ratio is dissolved in the water of formula ratio 1/2, obtains the jinggangmycin aqueous solution; The Avermectin of getting formula ratio is dissolved in the water of formula ratio 1/2, obtains the Avermectin aqueous solution; The sorbester p38 of formula ratio is dissolved in the atoleine of formula ratio, and is stand-by;
(4) add the water-soluble extract of tobacco leaf, the water-soluble extract of a sea red algae, the jinggangmycin aqueous solution and the Avermectin aqueous solution in the reactor, high speed shear 10 minutes, Tea Saponin adds in the high speed shear process, mixing also is warming up to 70～80 ℃, the Tween-60 that adds formula ratio, the high speed shear dispersion and emulsion;
(5) in reactor, add the atoleine that is dissolved with sapn that 1/3 step of measuring (1) obtains, high speed shear 10 minutes; Add the atoleine that is dissolved with sapn that 2/3 step of measuring (1) obtains again, high speed shear 30 minutes, regulating the pH value with the food-grade glacial acetic acid is 4.5, high pressure homogenizer 200kg/cm
2Homogeneous obtains described insecticidal spray EC.
Embodiment 3: the spray EC preparation
The raw material proportioning:
Atoleine 65%, jinggangmycin 2%, Avermectin 1%, Tea Saponin 2%, the water-soluble extract 0.6% of a sea red algae, the water-soluble extract 0.8% of tobacco leaf, sorbester p38 1.2%, Tween-60 0.4%, water 27%;
Method step:
(1) get a sea red algae 10kg, pulverize, 90 ℃ of extractings of water of 8 times of quality of adding 0.5 hour, centrifugal filtration gets extract I; Other gets a sea red algae 8kg, adds 8 times of extract I, and extracting is 30 hours under 90 ℃ of stirrings, and centrifugal filtration gets extract II, and extract II vacuum concentration to relative density is 1.05, and it is water-soluble, stand-by to get a described sea red algae extract;
(2) get dry tobacco leaf 10kg, pulverize, add 75 ℃ of extractings of water 1 hour of 9 times of quality, squeeze extract I; Other gets dry tobacco leaf 8kg, adds the extract I of 9 times of quality, and extracting is 2 hours under 75 ℃ of stirrings, squeeze extract II, extract II vacuum concentration to relative density is 1.06, the water-soluble extract of described tobacco leaf, stand-by;
(3) jinggangmycin of getting formula ratio is dissolved in the water of formula ratio 1/2, obtains the jinggangmycin aqueous solution; The Avermectin of getting formula ratio is dissolved in the water of formula ratio 1/2, obtains the Avermectin aqueous solution; The sorbester p38 of formula ratio is dissolved in the atoleine of formula ratio, and is stand-by;
(4) add the water-soluble extract of tobacco leaf, the water-soluble extract of a sea red algae, the jinggangmycin aqueous solution and the Avermectin aqueous solution in the reactor, high speed shear 10 minutes, Tea Saponin adds in the high speed shear process, mixing also is warming up to 70～80 ℃, the Tween-60 that adds formula ratio, the high speed shear dispersion and emulsion;
(5) in reactor, add the atoleine that is dissolved with sapn that 1/3 step of measuring (1) obtains, high speed shear 10 minutes; Add the atoleine that is dissolved with sapn that 2/3 step of measuring (1) obtains again, high speed shear 30 minutes, regulating the pH value with the food-grade glacial acetic acid is 4.5, high pressure homogenizer 200kg/cm
2Homogeneous obtains described insecticidal spray EC.
Embodiment 4: rat acute per os toxicity detects
The toxicity that embodiment 1～3 is made spray EC detects, and the results are shown in Table 1:
Table 1: insecticidal spray EC mouse acute oral toxicity (LD of the present invention
50)
| Embodiment | Test event | Test result (LD 50) |
| 1 | A) male, mg/KgBWt b) female, mg/KgBWt | ＞5000 ＞5000 |
| 2 | A) male, mg/KgBWt b) female, mg/KgBWt | ＞5000 ＞5000 |
| 3 | A) male, mg/KgBWt b) female, mg/KgBWt | ＞5000 ＞5000 |
The above results shows, the basic avirulence of insecticidal spray EC of the present invention.
Embodiment 5: the insecticidal activity test
Adopt the Potter spray-on process that embodiment 1～3 is made spray EC and carried out mythimna separata (Mythimnaseparata), black bean aphid (Aphis fabae), green rice leafhopper (Nephotettix cincticeps), two-spotted spider mite (Tetranchus urticae), the test of Tetranychus cinnabarinus (Tetranychus cinnabarinus) insecticidal activity.Test result sees Table 2.
Lethality is being the A level more than 90%, is the B level between 70～90%, is the C level between 50～70%, is the D level between 0～50%.
Table 2: insecticidal activity test effect
Conclusion: emulsion of the present invention has the broad spectrum disinfestation effect, the noresidue influence, and to people's environment and natural enemies security, duration of efficacy is longer.
Embodiment 6: the diseases prevention active testing
The spray EC that adopts toxic potato agar medium (PDA) method that embodiment 1～3 is prepared has carried out the bactericidal activity of Pyricularia oryzae (Pyricularia oryzae), fusarium graminearum (Gibberella zeae), Phytophthora capsici germ (Phytophthora capsici) and botrytis cinerea pers (Botrytis cinerea) to be measured, and general sieve concentration is 200 times of emulsions of dilution; The spray EC that adopts the toxic potato agar medium of excised leaf (PDA) method that embodiment 1～3 is prepared has carried out the bactericidal activity of Rhizoctonia solani Kuhn (Rhizoctonia solani) to be measured, and general sieve concentration is 200 times of emulsions of dilution; The spray EC that adopts potted plant toxic potato agar medium (PDA) method that embodiment 1～3 is prepared has carried out the bactericidal activity of Sclerotinia sclerotiorum (Sclerotonia sclerotiorum) to be measured, and general sieve concentration is 200 times of emulsions of dilution; The spray EC that adopts potted plant wheat seedling preservation spore method that embodiment 1～3 is prepared has carried out the bactericidal activity of wheat powdery mildew (Blumeria graminis) to be measured, and general sieve concentration is 200 times of emulsions of dilution.The bactericidal activity classification standard is divided: A level, preventive effect (inhibiting rate) 〉=95%; The B level, 70%≤inhibiting rate＜95%; The C level, 50%≤inhibiting rate＜70%; The D level, inhibiting rate＜50%.Test result sees Table 3.
Table 3: diseases prevention active testing effect
Conclusion (of pressure testing): find that through biological activity test the prepared spray EC of the present invention has certain bactericidal activity.
Embodiment 7: field control effectiveness test
Test in gross tea field, suburb, Fuyang, Hangzhou and carry out, soil property is a clay loam, middle fertility, and test mean temperature of air is 20～25 degrees centigrade.For trying insect: smaller green leaf hopper (false eye leafhopper Empoascaprisuga Matsumra, tea lesser leafhopper Empoasca flasvescems Feb.).Embodiment 1 gained missible oil extension rate is established 4 concentration gradients and is handled, and other establishes a clear water contrast.By above-mentioned 5 different disposal division of cells, each is handled 3 times and repeats during test, and district's group is arranged at random, totally 13 sub-districts, each sub-district area 25m
21000L calculates single subdistrict amount of liquid medicine, promptly every sub-district medication 2.5L by per hectare spray medicine.At dusk adopt workers and peasants' 16 type knapsack sprayers on May 17th, 2007, be sprayed on crop blade face, blade back and rhizome, but be as the criterion with firm dropping liquid; For processing mode A, 150 times of embodiment 1 gained missible oil dilutions are used in each sub-district; For processing mode B, 200 times of embodiment 1 gained missible oil dilutions are used in each sub-district, each sub-district; For processing mode C, 250 times of embodiment 1 gained missible oil dilutions are used in each sub-district, each sub-district; For processing mode D, 300 times of embodiment 1 gained missible oil dilutions are used in each sub-district, each sub-district; For processing mode E, clear water is used in each sub-district.
5 samplings of investigation method employing dish bat method great-jump-forward, promptly every some tea tray with diameter 35cm places tea fluffy down, pats tea fluffy 3 times with quick-moving speed, remaining worm alives and enumerates in full detail to shake and fall within the tea tray inside counting tea is fluffy.Respectively at observing the insect population number in 1 day, 5 days, 10 days, 30 days before the spray medicine and behind the spray medicine, calculate the insect population rate that goes down.
Residual borer population is as shown in table 4 after the preceding insect population cardinal sum dispenser of dispenser:
Table 4: field control effectiveness test effect
Conclusion (of pressure testing): the desinsection that the spray EC of the present invention preparation can be used for fruit tree, horticulture and flower, city trees and shrubs trees etc. has good prophylaxis effect simultaneously, and the lasting period is long, behind the medicine 30 days the time control efficiency still remarkable.
Embodiment 8: field control effectiveness test
(1) for studying thing and controlling object
For studying thing: a variety of Chinese cabbage kind is special short green vegetables (a Shanghai Long March vegetables seed companies), in the proving ground of sowing in the morning on April 27th, 2007 in the suburbs, Hangzhou, and field management such as applying fertilizer then, water, hoe up weeds.
(2) Toxicity Determination
Cabbage caterpillar low instar larvae: pick up from the proving ground in suburbs, Hangzhou on a variety of Chinese cabbage.Embodiment 3 gained missible oil extension rates are established 4 concentration gradients and are handled, each concentration of treatment triplicate, and other establishes a clear water contrast.Be that processing mode A uses 150 times of embodiment 1 gained missible oil dilutions for each sub-district; Processing mode B is that 200 times of embodiment 1 gained missible oil dilutions are used in each sub-district, each sub-district; Processing mode C is that 250 times of embodiment 1 gained missible oil dilutions are used in each sub-district, each sub-district; Processing mode D is that 300 times of embodiment 1 gained missible oil dilutions are used in each sub-district, each sub-district; Processing mode E uses clear water for each sub-district.Totally 13 processing are tested on May 12nd, 2007 and are carried out.
Adopt spray-on process, the clean back of drying of a variety of Chinese cabbage leaf is inserted for 15 of examination worms, above-mentioned various diluted concentration liquid portamist even spraying with embodiment 3 gained missible oil, polypide and blade are all touched for reagent liquid, observed result after blade behind the spray medicine was preserved moisture 1 day and 3 days is in right amount added up dead borer population.
(3) result of the test
Residual borer population is as shown in table 5 after the preceding insect population cardinal sum dispenser of dispenser:
Table 5: field control effectiveness test effect
(4) conclusion (of pressure testing): obvious in the prepared 300 times of diluted concentrations of spray EC of the present invention to the drug effect of cabbage caterpillar, therefore can be widely used in the controls of insect of plants such as fruits and vegetables.
Embodiment 9: the missible oil of embodiment 2 preparations and the compound use of other insect disinfestation component
Because the use for many years of chemical pesticides such as dimehypo, Hostathion, on the Rice Production harm loss the most serious insect---the pesticide resistance of striped rice borer obviously strengthens, cause the conventional pesticide preventive effect to descend.Missible oil and other insect disinfestation component of embodiment 2 preparations are composite, have the synergy of efficiently controlling snout moth's larva.Result of the test is as follows.
(1) test is handled
Different medicament comparative trials: establish every 666.7m
2Execute 20% triazophos emulsifiable solution (Xianju, Zhejiang insecticide factory) 100ml, 18% dimehypo water solution (Anhui and county insecticide factory) 400ml, 200 times of emulsions of missible oil dilution of embodiment 2 preparations, 400 times of emulsions of missible oil dilution of embodiment 2 preparations and the mixed liquor of Hostathion 50ml, and 400 times of emulsions of missible oil dilution of embodiment 2 preparations and the mixed liquor of dimehypo 200ml, other establishes spray clear water blank, amounts to 6 processing.
Test is all carried out in Xindeng, Fuyang town, and every processing repeats randomized arrangement 3 times.Different medicament comparative trials sub-district area is 50m
2For the rice varieties that tries the water is early rice Zhejiang 733, and the dispenser date is May 10 (the 1st a striped rice borer low instar larvae Sheng phase in generation), uses the knapsack sprayer even spraying, every 666.7m
2Dispenser liquid 50kg, the mud ridge is built in the minizone, not draining of 7d after the dispenser, does not pour water.
(2) investigation method
3d and 7d behind the medicine, 100 strain insect bite strains are looked in the stripping of every sub-district, and investigation striped rice borer lethality the results are shown in Table 6.
Table 6: different chemical control striped rice borer effects
(3) conclusion (of pressure testing): the spray EC of the present invention's preparation and the compound use of other insect disinfestation component have the synergy of efficiently controlling snout moth's larva, and its pesticide resistance are descended obviously.
Claims (6)
1. insecticidal spray EC mainly is made into by the following component of mass content:
Atoleine 40～65%
Jinggangmycin 2～5%
Avermectin 1～3%
Tea Saponin 2～10%
The water-soluble extract 0.5～2% of a sea red algae
The water-soluble extract 0.5～6% of tobacco leaf
Emulsifier 1.5～3%
Surplus is a water;
Described emulsifier is sapn and 3: 1 mixture of tween mass ratio.
2. insecticidal spray EC as claimed in claim 1, it is characterized in that the described sea water-soluble extract of a red algae is made by following method: get and do a sea red algae, pulverize, 80～100 ℃ of extractings of water of 8～10 times of quality of adding 0.5～2 hour, centrifugal filtration gets extract I; Other gets a sea red algae, adds the extract I of 8～10 times of quality, and extracting is 24～36 hours under 90～100 ℃ of stirrings, and centrifugal filtration gets extract II, and extract II vacuum concentration to relative density is 1.05～1.15, gets the water-soluble extract of a described sea red algae.
3. insecticidal spray EC as claimed in claim 1 is characterized in that the water-soluble extract of described tobacco leaf is made by following method: get dry tobacco leaf, pulverize, add 70～80 ℃ of extractings of water 1～2 hour of 8～10 times of quality, squeeze extract I; Other gets dry tobacco leaf, adds the extract I of 8～10 times of quality, and extracting is 2～4 hours under 70～80 ℃ of stirrings, squeeze extract II, extract II vacuum concentration to relative density is 1.05～1.15, the water-soluble extract of described tobacco leaf.
4. insecticidal spray EC as claimed in claim 1 is characterized in that described sapn is a sorbester p38, and described tween is a Tween-60.
5. preparation is as the method for insecticidal spray EC as described in one of claim 1～4, the main raw materials in proportion for preparing described insecticidal spray EC is: atoleine 40～65%, jinggangmycin 2～5%, Avermectin 1～3%, Tea Saponin 2～10%, a sea red algae extract 0.5～2%, tobacco leaf extract 0.5～6%, emulsifier 1.5～3%, surplus are water; Described emulsifier is sapn and 3: 1 mixture of tween mass ratio; Described method comprises:
(1) jinggangmycin of getting formula ratio is dissolved in the water of formula ratio 1/3～2/3, obtains the jinggangmycin aqueous solution; The Avermectin of getting formula ratio is dissolved in the water of formula ratio 1/3～2/3, obtains the Avermectin aqueous solution; The sapn of formula ratio is dissolved in the atoleine of formula ratio, and is stand-by;
(2) add the water-soluble extract of tobacco leaf, the water-soluble extract of a sea red algae, the jinggangmycin aqueous solution and the Avermectin aqueous solution in the reactor, in high speed shear, add Tea Saponin, mixing also is warming up to 70～80 ℃, adds the tween of formula ratio, the high speed shear dispersion and emulsion;
(3) in reactor, add the atoleine that is dissolved with sapn that 1/3 step of measuring (1) obtains, high speed shear 10～15 minutes; Add the atoleine that is dissolved with sapn that 2/3 step of measuring (1) obtains again, high speed shear 25～30 minutes, it is 4.5 that glacial acetic acid is regulated the pH value, 200kg/cm
2Homogeneous obtains described insecticidal spray EC.
6. method as claimed in claim 5, it is characterized in that: the main raw materials in proportion for preparing described insecticidal spray EC is: atoleine 50%, jinggangmycin 3%, Avermectin 2%, Tea Saponin 6%, a sea red algae extract 1%, tobacco leaf extract 4%, sorbester p38 1.5%, Tween-60 0.5%, water 32%; Described method is as follows:
(1) get a sea red algae, pulverize, 90 ℃ of extractings of water of 10 times of quality of adding 0.5 hour, centrifugal filtration gets extract I; Other gets a sea red algae, adds the extract I of 10 times of quality, and extracting is 30 hours under 90 ℃ of stirrings, and centrifugal filtration gets extract II, and extract II vacuum concentration to relative density is 1.05, gets the water-soluble extract of a described sea red algae, and is stand-by;
(2) get dry tobacco leaf, pulverize, add 75 ℃ of extractings of water 1 hour of 8 times of quality, squeeze extract I; Other gets dry tobacco leaf, adds the extract I of 8 times of quality, and extracting is 2 hours under 75 ℃ of stirrings, squeeze extract II, extract II vacuum concentration to relative density is 1.05, the water-soluble extract of described tobacco leaf, stand-by;
(3) jinggangmycin of getting formula ratio is dissolved in the water of formula ratio 1/2, obtains the jinggangmycin aqueous solution; The Avermectin of getting formula ratio is dissolved in the water of formula ratio 1/2, obtains the Avermectin aqueous solution; The sorbester p38 of formula ratio is dissolved in the atoleine of formula ratio, and is stand-by;
(4) add the water-soluble extract of tobacco leaf, the water-soluble extract of a sea red algae, the jinggangmycin aqueous solution and the Avermectin aqueous solution in the reactor, in high speed shear, add Tea Saponin, mixing also is warming up to 70～80 ℃, adds the Tween-60 of formula ratio, the high speed shear dispersion and emulsion;
(5) in reactor, add the atoleine that is dissolved with sapn that 1/3 step of measuring (1) obtains, high speed shear 10 minutes; Add the atoleine that is dissolved with sapn that 2/3 step of measuring (1) obtains again, high speed shear 30 minutes, regulating the pH value with glacial acetic acid is 4.5,200kg/cm
2Homogeneous obtains described insecticidal spray EC.
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| CN107156209A (en) * | 2017-05-25 | 2017-09-15 | 乐清瑞耀食品技术有限公司 | Method for producing insecticide for the greenhouse water spinach prevention and control of plant diseases, pest control |
| MA60456B1 (en) * | 2023-05-22 | 2025-02-28 | Universite Mohammed VI Polytechnique | Bio-insecticide based on red algae for the fight against cochineal, its preparation and use |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1234972A (en) * | 1998-05-08 | 1999-11-17 | 珠海绿色南方保鲜总公司 | Agent for killing mite and pest |
| CN1267451A (en) * | 1999-03-23 | 2000-09-27 | 王玉万 | Mineral oil-containing pesticide for protecting plant |
| WO2006126211A2 (en) * | 2005-05-27 | 2006-11-30 | Indian Oil Corporation Limited | Composition of an agricultural spray oil |
| CN101032256A (en) * | 2007-04-13 | 2007-09-12 | 彭国均 | Pesticide of composite jinggangmycin |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1234972A (en) * | 1998-05-08 | 1999-11-17 | 珠海绿色南方保鲜总公司 | Agent for killing mite and pest |
| CN1267451A (en) * | 1999-03-23 | 2000-09-27 | 王玉万 | Mineral oil-containing pesticide for protecting plant |
| WO2006126211A2 (en) * | 2005-05-27 | 2006-11-30 | Indian Oil Corporation Limited | Composition of an agricultural spray oil |
| CN101032256A (en) * | 2007-04-13 | 2007-09-12 | 彭国均 | Pesticide of composite jinggangmycin |
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