CN103814964B - A kind of emulsion for killing aphid and two spotted spider mite and preparation method thereof - Google Patents
A kind of emulsion for killing aphid and two spotted spider mite and preparation method thereof Download PDFInfo
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- CN103814964B CN103814964B CN201410054908.0A CN201410054908A CN103814964B CN 103814964 B CN103814964 B CN 103814964B CN 201410054908 A CN201410054908 A CN 201410054908A CN 103814964 B CN103814964 B CN 103814964B
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Abstract
The invention discloses a kind of emulsion for killing aphid and two spotted spider mite and preparation method thereof.This emulsion with tree-of-heaven leaf the water extracted immersing paste, kuh-seng alcohol-extracted extract, folium cortex eucommiae the water extracted immersing paste, amargosa alcohol-extracted extract composition mixing medicinal extract for main ingredient, in main ingredient, the weight ratio of four kinds of medicinal extract is 1: 1: 2: 2, also comprises the component of following consumption in this emulsion relative to every gram of main ingredient: solvent 40 ~ 50mL, emulsifier 5 ~ 15mL, auxiliary agent 0.05 ~ 0.15g, preservative 1 ~ 2mL, antifreezing agent 5 ~ 7.5mL, deionized water 50 ~ 100mL.The preparation method of this emulsion is: four kinds of medicinal extract mix by (1) in proportion, add solvent, heating for dissolving, obtain liquid; (2) in liquid, add emulsifier and auxiliary agent, utilize ultrasonic emulsification device to obtain primary emulsion; (3) in primary emulsion, slowly drip preservative, antifreezing agent and deionized water successively, stir, be down to room temperature and get final product.Environmental friendliness of the present invention, steady quality, good disinsection effect, preparation method's technological operation is simple, and production cost is low.
Description
Technical field
The present invention relates to a kind of emulsion for killing aphid and two spotted spider mite and preparation method thereof, belonging to natural plants applied technical field.
Background technology
The world today faces four problems, i.e. population problem, food problem, energy problem and environmental problem.China's crops main diseases and insect pests has kind more than 1500, especially severe have tens kinds.Up to now, chemical control remains topmost means and measure in China's pest management.Wherein more than 95% use chemical pesticide, biopesticide proportion is only 2% ~ 3%, and emulsion is very few especially.Agricultural chemicals is being killed, is being suppressed damage by disease and insect on the one hand, ensures to play a very important role in crops high and stable yields, meanwhile, also can jeopardize the safety of environment due to irrational use thus by all means, and then infringement health.The high poison of China, highly toxic pesticide kind are in the majority, extremely serious pollution has been caused to environment, agricultural chemicals residual quantity in food agricultural produce exceeds the corresponding standard of country on a large scale, and have the trend continuing to increase, serious infringement and impact are constituted on the physical and mental health of the common people and export of farm produce trade.
Plant resource in biogenic substances agricultural chemicals, microbial pesticide proportion are relatively larger, are that the important of New pesticides discovery is first had its source.For many years by the developmental research to plant resources, find that the floristics that can become agricultural chemicals is a lot, mainly concentrate on the sections more than 30 such as Meliaceae, composite family, pulse family, Celastraceae, Euphorbiaceae.The active substance related generally to is: 1. glucosides class (as gleditsin Aglycone, crotons glucosides, tomatin); 2. phenols and quinones (as gossypol, Walnut Leaves quinone and shrubby flase indigo element); 3. alkaloids (as nicotine, wilfordine); 4. terpene (as firpene, live that happy wood is normal, toosendanin and nimbin); 5. steroid class (as ponasterone and Inokosterone).Therefore, prepare effective, the non-environmental-pollution of pest control, noresidue biopesticide significant.
People have done large quantity research for insecticide emulsion.The people such as Miao Kang, Shu Zhaolin study with 25% first dimension chlorpyrifos aqueous emulsion the control efficiency of wheat aphid, adopt emamectin-benzoate 0.2%, chlopyrifos 24.8%, built agent controls wheat aphid and all plays an important role in Wheat Production, and field trial shows: 25% first dimension chlorpyrifos aqueous emulsion control wheat aphid has the advantage that quick-acting is good, the lasting period is long.1 ~ 3d after medicine, 25% first dimension chlorpyrifos aqueous emulsion various dose is 93.48% ~ 100% (Jiangsu's agriculture science, 2010,6:199-200) to the control efficiency of wheat aphid.The people such as Qin Guicong, Cen Liujun adopt and to kill precious aqueous emulsion more 4% and add the test of pesticide effectiveness of the new synergist of 0.5%-3% to vegetables cabbage caterpillar and aphid, result shows: 24h after medicine, the Revision insect recluced rate of aphid improves 2.27% (Guangxi Agricultural science, 2007,3:167-168).The people such as Cheng Hongsen study the controlling experiment of different miticide to Chinese rose of cut flower two spotted spider mite, find that propargite 1500 times of dilutions are a kind of favourable agents (Agriculture of Anhui science, 2008,36:10536-10537) preventing and treating two spotted spider mite.The people such as Sun Meimei, Chai Weigang study the control action of 8 Plant Extracts to two spotted spider mite, and toxicity result of the test shows: garlic P.E is better to the repellent action of Tetranychus cinnabarinus, and after medicine, 1d scattering ratio reaches 88.21%; Tea seed cake extract is better to Tetranychus cinnabarinus toxic action, and after medicine, 3d lethality can reach 90.07%.Field control effectiveness test result shows: garlic and tea seed cake 2 kinds of extracts have certain control effects to two spotted spider mite, but its lasting effect poor (Ningbo agricultural science and technology, 2011,2:13-15).The people such as Zhao Baitao carry out total alkaloid from sophora flavescens ait optimal extraction technology and killing aphids activity research, by shrubby sophora extract, the test of the insecticidal activity assay of aphid is shown, different disposal is carried out to Radix Sophorae Flavescentis extractive liquid and with its insecticidal activity significant difference of different solvents; Take chloroform as Extraction solvent, gained total alkaloid from sophora flavescens ait content is the highest, and its insecticidal activity is the highest; Take ethanol as Extraction solvent, chloroform extract is compared with concentrate, when same concentrations total alkaloids, chloroform extract is higher to aphid insecticidal activity, may be that in ethanol concentrate, impurities is more, interference (Chinese Wild plant resources is caused to total alkaloids insecticidal activity, 2008,27 (1): 43-46).
Patent document CN102578164A discloses a kind of plant source compound Synergistic insecticidal containing matrine and Macleaya cordata alkaloids and preparation method thereof, this obtained Botanical synergistic compound pesticide is main component and adds additive compound to form by matrine and Macleaya cordata alkaloids, and dosage form is environment-friendly type missible oil, aqua or soluble liquid; Containing matrine 0.1% ~ 20% in preparation, Macleaya cordata alkaloids 0.1% ~ 20%, all the other are auxiliary agent.Be mainly used in control melon, pest such as aphid, two spotted spider mite, fragrant-flowered garlic maggot, Paratrioza sinica, pear sucker, cabbage caterpillar, diamond-back moth, mythimna separata really, on vegetables.Patent document CN102524271A discloses sparteine matrine disinsection aqueous emulsion, this sparteine matrine disinsection aqueous emulsion is 15% ~ 20% by the consumption of sparteine extract and the composite aqueous emulsion of matrine extract wherein sparteine extract, its every 1 milliliter of liquid is equivalent to 2 grams of crude drugs, the consumption of matrine extract is 8% ~ 10%, its 1 every milliliter of liquid is equivalent to 2 grams of crude drugs, and above-mentioned consumption is with volume percentage.This invention by sparteine and the mixing of matrine two Plants source alkaloid, thus obtains efficient, low toxicity and the little biopesticide of environmental pollution.The main components such as the sparteine that this invention is used and matrine are all the natural productss extracted from plant, and sparteine and matrine have insecticidal action, therefore have very strong killing action to insect.Patent document CN101843262A discloses and a kind ofly prevents and treats agricultural chemicals of melon or fruit type crops aphid and two spotted spider mite and preparation method thereof, the composition of raw materials of this invention is castor oil 27.5-37.5 part, solvent 20-50 part, emulsifier 15-30 part, bleeding agent 0.5-3 part, antifreeze 1-5 part, castor seeds is pulverized, added solvent, Soakage extraction repeatedly merges extract afterwards, hydraulic pressure is concentrated into after solvent is evaporated completely and obtains castor oil mother liquor, in castor oil mother liquor, add dissolution with solvents again, after add emulsifier, bleeding agent and antifreeze, namely obtain castor oil emulsion finished product after mixing.This invention processing technology is simple, and with low cost, quick-acting is good, the lasting period is long, significantly can reduce access times and the using dosage of chemical pesticide, effectively reduces the persticide residue in melon dish, preserves the ecological environment, promote agricultural product quality and safety.
A kind of agricultural chemicals for killing aphid and two spotted spider mite and preparation method thereof disclosed in patent document CN102125061A, the method is effective component extracting from natural plants tree-of-heaven leaf, folium cortex eucommiae and kuh-seng, is mixed with agricultural chemicals, can be used for killing aphid, two spotted spider mite.The method of this invention is first effective component extracting from tree-of-heaven leaf, folium cortex eucommiae and kuh-seng, Radix Sophorae Flavescentis extractive liquid obtains matrine through HZ801 type resin separation purification, the extraction concentrate of tree-of-heaven leaf, folium cortex eucommiae mixes with matrine compatibility, prepares that deinsectization persistent, production cost are low, the simple natural green agricultural chemicals of technological operation.
Summary of the invention
The object of the present invention is to provide a kind of new emulsion for killing aphid and two spotted spider mite, this emulsion environmental friendliness, steady quality, good disinsection effect.
Another object of the present invention is to the preparation method providing a kind of described emulsion, the method is simple to operate, and production cost is low.
For achieving the above object, the present invention is by the following technical solutions:
For killing an emulsion for aphid and two spotted spider mite, this emulsion is with the mixing medicinal extract of tree-of-heaven leaf the water extracted immersing paste, kuh-seng alcohol-extracted extract, folium cortex eucommiae the water extracted immersing paste, amargosa alcohol-extracted extract composition for main ingredient, and in main ingredient, the weight ratio of four kinds of medicinal extract is 1: 1: 2: 2.
The component of following consumption is also comprised relative to every gram of main ingredient: solvent 40 ~ 50mL, emulsifier 5 ~ 15mL, auxiliary agent 0.05 ~ 0.15g, preservative 1 ~ 2mL, antifreezing agent 5 ~ 7.5mL, deionized water 50 ~ 100mL in described emulsion.
Wherein, described solvent is n-hexane, dimethylbenzene, cyclohexanone, cyclohexanol or 200# solvent naphtha.Described emulsifier is polysorbas20, polysorbate60, polysorbate65, Tween 80 or polysorbate85.Described auxiliary agent is sodium carboxymethylcellulose.Described preservative is the ethanolic solution containing 5%g/mL ethylparaben.Described antifreezing agent is the aqueous solution of the ethylene glycol containing 5%g/mL.
Wherein, the preparation method of four kinds of medicinal extract such as tree-of-heaven leaf the water extracted immersing paste, kuh-seng alcohol-extracted extract, folium cortex eucommiae the water extracted immersing paste, amargosa alcohol-extracted extract is as follows:
Tree-of-heaven leaf the water extracted immersing paste: put into extractor after being pulverized by tree-of-heaven leaf, add the water of 4 times of weight wherein, add hot reflux 2h, add a small amount of ethanol, after alcohol precipitation, filters, filtrate is concentrated into medicinal extract, is cooled to 4 DEG C of preservations stand-by;
Kuh-seng alcohol-extracted extract: kuh-seng is put into extractor, adds 50% ethanol of 4 times of weight wherein, adds hot reflux 2h, and filter, filtrate is concentrated into medicinal extract, is cooled to 4 DEG C of preservations stand-by;
Folium cortex eucommiae the water extracted immersing paste: put into extractor after being pulverized by folium cortex eucommiae, add the water of 3 times of weight wherein, add hot reflux 2h, add a small amount of ethanol, after alcohol precipitation, filters, filtrate is concentrated into medicinal extract, is cooled to 4 DEG C of preservations stand-by;
Amargosa alcohol-extracted extract: put into extractor after being pulverized by amargosa, add 50% ethanol of 3 times of weight wherein, add hot reflux 2h, filter, filtrate is concentrated into medicinal extract, is cooled to 4 DEG C of preservations stand-by.
A preparation method for the described emulsion for killing aphid and two spotted spider mite, comprises the following steps:
(1) tree-of-heaven leaf the water extracted immersing paste, kuh-seng alcohol-extracted extract, folium cortex eucommiae the water extracted immersing paste, amargosa alcohol-extracted extract are mixed in proportion, add solvent, in 30 ~ 50 DEG C of heating for dissolving, obtain liquid;
(2) in the liquid obtained, add emulsifier and auxiliary agent, utilize ultrasonic emulsification device, supersonic frequency is 10 ~ 15kHz, and ultrasonic time is 30 ~ 60min, and temperature is 50 ~ 70 DEG C, obtains primary emulsion;
(3) in primary emulsion, preservative, antifreezing agent and deionized water is slowly dripped successively, rate of addition is 2 ~ 5mL/min, in 40 ~ 60 DEG C of heating water baths, stir with 5000 ~ 8000r/min simultaneously, continue stirring 20 ~ 30min after dripping deionized water, stopping stirring, being slowly down to the faint yellow emulsion that namely room temperature obtains for killing aphid and two spotted spider mite, sealing, puts shady and cool place storage.
The invention has the advantages that:
The present invention, on early-stage Study basis, concentrates plant pesticide extract, makes medicinal extract, be then prepared into aqueous emulsion.The present invention uses a small amount of organic solvent, take water as continuous phase, and Liquid Insecticides is disperse phase, can suppress the volatilization of insecticide, avoid or reduces organic solvent to the toxicity of people and animals and excitant.Emulsion steady quality of the present invention, kill the liquid preparation that aphid, two spotted spider mite effect are better than chemical pesticide and above-mentioned formulation of pesticide in 7 days, preparation method's technological operation of the present invention is simple, production cost is low, utilize preparation method of the present invention can obtain deinsectization persistent, pest control is effective, non-environmental-pollution, noresidue, the natural green agricultural chemicals of environment-friendly type.
Embodiment
The invention will be further described by the following examples, but the present invention is not limited to following examples.
The present invention adopts tree-of-heaven leaf, folium cortex eucommiae, amargosa and kuh-seng to be raw material, wherein tree-of-heaven, has another name called Ailanthus altissima or wood rice huller tree, the ancient title tree of heaven.Having item wood, is Simarubaceae deciduous tree plant.Gain the name because leaf base gland point disperses stink.To the better resistance of flue dust and sulphur dioxide, damage by disease and insect is less.Can be drought-resistant and saline and alkaline, and growth is fast, can make city, industrial and mining area and rural area green tree species, widely distributed in China.Tree-of-heaven is the strongest to tobacco mosaic virus inhibitory action, and to cucumber mosaic virus, marmor upsilon has significant external inhibit activities, has the potentiality that exploitation becomes plant antiviral agent.Form: deciduous tree, Gao Keda 30 meters, tree crown is oblate spheroid or umbrella shape.Bark canescence or grey black, smoothly, slightly checking.Sprig is sturdy.Leaf scar is large, obovate, interior tool 9 bundle scars.Imparipinnate leaf, alternate, leaflet 13-25 piece, ovum shape lanceolar, the full edge in middle and upper part, nearly base portion has 1-2 to rough sawn tooth, and tooth top has gland point, and leaf footstalk base portion expands, frowziness.The 5-6 month blooms, and panicle top is raw, and floral white is micro-smelly.Capsule is oval, and seed is most, has the wing of flat film quality.
The bark of eucommia, another name silk cotton tree, silk flosssilk wadding skin, beautiful silk skin.Folium cortex eucommiae contains the active ingredient the same with Bark of Eucommia Ulmoides, and the medicinal active ingredient of greenery is higher than bark.Folium cortex eucommiae contains multiple medicinal ingredient, as β-D-Glucose glucoside, chlorogenic acid, Aucubin.The place of production is distributed more widely general, mainly originates in the ground such as Sichuan, Shaanxi, Hubei, Henan, Guizhou, Yunnan.Form: deciduous tree, up to 20m.Bark taupe, coarse, fracture and pulled open most filament.Sprout has yellowish-brown hair, and rear change is without hair, and old branch has hole skin.Single leaf alternate; The long 1-2cm of petiole, has groove above, is become mildewed by scattered; Oval, the avette or Long Circle of blade, long 6-15cm, wide 3.5-6.5cm, tip is gradually sharp, basal circular or wealthy wedge shape, above dirty-green, below pale green, Lao Ye is wrinkle slightly, and there is sawtooth at edge; Lateral vein 6-9 couple.Flower unisexuality, dioecism, peanut is in current growth base portion, and male flower is without perianth, and bennet is without hair; Stamen is about 1cm, without hair, without pistillode; Female flower Dan Sheng, bennet is about 8mm, ovary 1 Room, and tip 2 splits, and ovary handle is extremely short.Samara is flat, oblong, and tip 2 splits, base portion wedge shape, around the thin wing of tool; Nut is positioned at central authorities, has joint with carpopodium joint.Early spring blooms, after autumn fruit maturation.
Kuh-seng another name matrine, chuanshentong, phoenix claw, Niu Can etc., derive from the root of leguminous plant kuh-seng, all parts of the country are all produced, function heat-clearing, eliminating dampness, desinsection etc.Main component in kuh-seng is matrine, and chemical constitution is the quinolizine pyridine all with Fourth Ring.Source: this product is the dry root of leguminous plant kuh-seng.Spring, Qiu Erji excavate, removing root head and little supporting root, cleaning, drying, or take advantage of fresh slices, dry.Proterties: this product is elongated cylindrical, and often there is branch bottom, long 10 ~ 30cm, diameter 1 ~ 2cm.Surface taupe brown or brown color, tool indulges wrinkle and hole skin of growing crosswise.Crust is thin, and break warp more, easily peels off, and exfoliation displaing yellow is smooth.Matter is hard, not frangibility, section fibrous.Slice thick 3 ~ 6mm; Tangent plane yellow-white, the radial texture of tool and crack, the visible proper alignment ring grain had.Gas is micro-, and taste is extremely bitter.
The Ji Yuan of medicinal material melia is bark and the root skin of Meliaceae plant melia toosendan, chinaberry deciduous tree, high 15-20m.Bark crineous, lobe, old branch purple, has most tiny hole skin.Two to three times imparipinnate leaf alternates, are born in wilderness or roadside, often cultivate after room anterior chamber.Distribution north, to Hebei, reaches Guangxi, Yunnan in the south, to Sichuan and other places.Containing toosendanin (toosendanin) in Neem bark, China tree ketone (kulinone), China tree terpene ketone lactone (kulactone), China tree terpene alcoholic lactone.Nature and flavor: bitter; Cold; Poisonous.Function cures mainly: have ascarifuge, in pinworm and whip.As a kind of plant insecticide be separated from Meliaceae and the branch skin of China tree, there is stomach toxicity, tag and certain Antifeedant Effects.
Tree-of-heaven leaf used in the present invention is plucked in Biochemical Engineering College of Beijing Union University's garden with hundreds of grasses, plucking time is annual summer, folium cortex eucommiae is plucked in Anguo Biochemical Engineering College of Beijing Union University, Hebei Practical Teaching Base, plucking time is annual summer, dry kuh-seng and be purchased from the careless Co., Ltd in Xuancheng hundred, amargosa is purchased from Anguo traditional Chinese medicine trade market.
Four kinds of medicinal extract such as tree-of-heaven leaf the water extracted immersing paste used in the present invention, kuh-seng alcohol-extracted extract, folium cortex eucommiae the water extracted immersing paste, amargosa alcohol-extracted extract are prepared in accordance with the following methods:
Tree-of-heaven leaf the water extracted immersing paste: put into extractor after being pulverized by tree-of-heaven leaf, add the water of 4 times of weight wherein, add hot reflux 2h, add a small amount of ethanol, after alcohol precipitation, filters, filtrate is concentrated into medicinal extract, is cooled to 4 DEG C of preservations stand-by;
Kuh-seng alcohol-extracted extract: kuh-seng is put into extractor, adds 50% ethanol of 4 times of weight wherein, adds hot reflux 2h, and filter, filtrate is concentrated into medicinal extract, is cooled to 4 DEG C of preservations stand-by;
Folium cortex eucommiae the water extracted immersing paste: put into extractor after being pulverized by folium cortex eucommiae, add the water of 3 times of weight wherein, add hot reflux 2h, add a small amount of ethanol, after alcohol precipitation, filters, filtrate is concentrated into medicinal extract, is cooled to 4 DEG C of preservations stand-by;
Amargosa alcohol-extracted extract: put into extractor after being pulverized by amargosa, add 50% ethanol of 3 times of weight wherein, add hot reflux 2h, filter, filtrate is concentrated into medicinal extract, is cooled to 4 DEG C of preservations stand-by.
Embodiment 1
Tree-of-heaven leaf the water extracted immersing paste, kuh-seng alcohol-extracted extract, folium cortex eucommiae the water extracted immersing paste, amargosa alcohol-extracted extract are mixed to get 2.0g mixing medicinal extract according to weight ratio 1: 1: 2: 2, add (or dimethylbenzene, cyclohexanone, cyclohexanol, 200# solvent naphtha) in n-hexane, in 40 DEG C of heating for dissolving, obtain liquid; Join in the liquid of configuration according to the amount of prescription 1 by emulsifier tween 80 and auxiliary agent sodium carboxymethylcellulose, utilize ultrasonic emulsification device, supersonic frequency is 15kHz, and ultrasonic time is 30min, temperature is 60 DEG C, obtains primary emulsion; Slowly the ethylparaben of 5%g/mL, the ethylene glycol solution of 5%g/mL and deionized water is dripped in primary emulsion, rate of addition is 3mL/min, in 60 DEG C of heating water baths, stir with 7000r/min simultaneously, continue to stir 30min after dripping deionized water, answer slow cooling after emulsion is formed, should not stir during cooling, to prevent drop from assembling, namely obtain the faint yellow emulsion killing aphid and two spotted spider mite.The selection of solvent on gained solvent stability to affect result as shown in table 1.
prescription 1
Table 1 solvent affects emulsion stability
| Solvent | Particle diameter (nm) | Emulsion outward appearance |
| N-hexane | 168.34±87.49 | Long-term placement does not have layering |
| Dimethylbenzene | 178.52±59.37 | Long-term placement does not have layering |
| Cyclohexanone | 197.28±93.57 | Place and have lamination in 60 days |
| Cyclohexanol | 194.32±47.39 | Place and have lamination in 37 days |
| 200# solvent naphtha | 204.18±68.39 | Place and have lamination in 40 days |
Embodiment 2
Tree-of-heaven leaf the water extracted immersing paste, kuh-seng alcohol-extracted extract, folium cortex eucommiae the water extracted immersing paste, amargosa alcohol-extracted extract are mixed to get 2.0g mixing medicinal extract according to weight ratio 1: 1: 2: 2, add in n-hexane solvent, in 40 DEG C of heating for dissolving, obtain liquid; According to the amount of prescription 2, emulsifier tween 60 (or Tween 80) and auxiliary agent sodium carboxymethylcellulose are joined in the liquid of configuration, utilize ultrasonic emulsification device, supersonic frequency is 15kHz, and ultrasonic time is 30min, temperature is 60 DEG C, obtains primary emulsion; Slowly the ethylparaben of 5%g/mL, the ethylene glycol solution of 5%g/mL and deionized water is dripped in primary emulsion, rate of addition is 3mL/min, in 60 DEG C of heating water baths, stir with 7000r/min simultaneously, continue to stir 30min after dripping deionized water, answer slow cooling after emulsion is formed, should not stir during cooling, to prevent drop from assembling, namely obtain the faint yellow emulsion killing aphid and two spotted spider mite.
The mensuration of Zeta potential adopts electrophoretic light scattering method to measure.Light source: HeNe laser (λ
0=633nm); Medium: water (n=1.33); Electric potential gradient: E=10V/cm; Angle of scattering: θ=9 °; Measure temperature: 20 DEG C.Precision measures emulsion 50 μ L in 50mL measuring bottle, is diluted to scale with pure water, gets the zeta current potential that appropriate solution measures emulsion in sample cell.The selection of emulsifier on gained emulsion stability to affect result as shown in table 2.
prescription 2
Table 2 emulsifier affects emulsion stability
| Emulsifier (mL) | Vzeta(mV) |
| Polysorbas20 | -10.21 |
| Polysorbate60 | -12.75 |
| Tween 80 | -16.73 |
Adopt emulsifier tween 80, zeta current potential absolute value comparatively large in prescription, its interparticle electrostatic repulsion is also larger, and physical stability is also better.In order to observe the layering of emulsion at short notice, centrifugal process is adopted to accelerate its layering.With the centrifugal 15min of 4000r/min, not stratified, emulsion steady quality.
Embodiment 3
According to following formula preparation agricultural-chemical emulsion I:
II: get in 75% DDT EC 1mL to 2000mL tun, adding distil water is diluted to 1500mL;
III: get in 48% omethoate emulsifiable solution 1mL to 2000mL tun, adding distil water is diluted to 1500mL;
IV: clear water.
Do the efficiency test in three seasons continuously, each season is parallel does three times, investigates agricultural-chemical emulsion of the present invention (I), dichlorvos (II) and flolimat (III) to the control efficiency of aphid, two spotted spider mite.Experimental result is as shown in Table 3, 4:
Table 33 kind of insecticide is to the control efficiency of aphid
Table 43 kind of insecticide is to the control efficiency of two spotted spider mite
Wherein:
Test shows: agricultural-chemical emulsion of the present invention was all better than chemical pesticide to the preventive effect of aphid, two spotted spider mite from the 3rd day; Still be greater than 80% by the 7th day to the Rectifying efficacies of aphid, be greater than 75% to the Rectifying efficacies of two spotted spider mite, lasting effect is better; The cost accounting data of test agricultural chemicals are shown: this pesticide price is only 1.43 times of dichlorvos price, 1.37 times of flolimat.
Embodiment 4
Tree-of-heaven leaf the water extracted immersing paste, kuh-seng alcohol-extracted extract, folium cortex eucommiae the water extracted immersing paste, amargosa alcohol-extracted extract are mixed to get 2.0g mixing medicinal extract according to weight ratio 1: 1: 2: 2, add in n-hexane solvent, in 40 DEG C of heating for dissolving, obtain liquid; Join in the liquid of configuration according to the amount of prescription 3 by emulsifier tween 80 and auxiliary agent sodium carboxymethylcellulose, utilize ultrasonic emulsification device, supersonic frequency is 15kHz, and ultrasonic time is 30min, temperature is 60 DEG C, obtains primary emulsion; The ethylparaben of 5%g/mL, the ethylene glycol solution of 5%g/mL and deionized water is slowly dripped to colostrum, rate of addition is 3mL/min, in 60 DEG C of heating water baths, stir with 7000r/min simultaneously, continue to stir 30min after dripping deionized water, answer slow cooling after emulsion is formed, should not stir during cooling, to prevent drop from assembling, namely obtain the faint yellow emulsion killing aphid and two spotted spider mite.
prescription 3
According to current relevant national standard and FAO standard, HG/T2467.9-2003 " pesticide emulsion in water product standard writes specification ", works out quality control index, detects this insecticide emulsion quality.
1, microemulsion stability test
Carry out with reference to GB/T1603-2001 method, dilute 200 times, microemulsion sample standard hard water dilutes, 30 DEG C of constant volumes in volumetric flask, leave standstill 1h, observe microemulsion emulsion-stabilizing situation during this period, as nodeless mesh or oil slick, the oil that sinks are separated out, also there is not suspension or become muddy, then think that stability of emulsion is qualified.
2, low-temperature stability test
Being undertaken by GB/T19137-2003, take out, return to room temperature, through slowly shaking, separating out as qualified without visible solid particle or grease.
3, heat storage stability test
Undertaken by GB/T19136-2003.Test to gainer, its result still meets standard-required, be then qualified.
4, pourability test
After the sample being placed in container is placed certain hour, program is toppled over according to the rules, and measure the amount being trapped in sample in container, after being washed with water by container, then measure the sample size in container, this agricultural-chemical emulsion does target with matrine content.
Table 5 emulsion quality and technical index
Claims (4)
1. one kind for killing the emulsion of aphid and two spotted spider mite, it is characterized in that, this emulsion is with the mixing medicinal extract of tree-of-heaven leaf the water extracted immersing paste, kuh-seng alcohol-extracted extract, folium cortex eucommiae the water extracted immersing paste, amargosa alcohol-extracted extract composition for main ingredient, and in main ingredient, the weight ratio of four kinds of medicinal extract is 1:1:2:2;
The component of following consumption is also comprised relative to every gram of main ingredient: solvent 40 ~ 50mL, emulsifier 5 ~ 15mL, auxiliary agent 0.05 ~ 0.15g, preservative 1 ~ 2mL, antifreezing agent 5 ~ 7.5mL, deionized water 50 ~ 100mL in this emulsion;
Wherein, described emulsifier is polysorbas20, polysorbate60, polysorbate65, Tween 80 or polysorbate85; Described auxiliary agent is sodium carboxymethylcellulose; Described preservative is the ethanolic solution of 0.05g/mL ethylparaben; Described antifreezing agent is the aqueous solution of the ethylene glycol of 0.05g/mL.
2. the emulsion for killing aphid and two spotted spider mite according to claim 1, is characterized in that, described solvent is n-hexane, dimethylbenzene, cyclohexanone, cyclohexanol or 200# solvent naphtha.
3. the emulsion for killing aphid and two spotted spider mite according to claim 1, is characterized in that, the preparation method of described four kinds of medicinal extract is:
Tree-of-heaven leaf the water extracted immersing paste: put into extractor after being pulverized by tree-of-heaven leaf, add the water of 4 times of weight wherein, add hot reflux 2h, add a small amount of ethanol, after alcohol precipitation, filters, filtrate is concentrated into medicinal extract, is cooled to 4 DEG C of preservations stand-by;
Kuh-seng alcohol-extracted extract: kuh-seng is put into extractor, adds 50% ethanol of 4 times of weight wherein, adds hot reflux 2h, and filter, filtrate is concentrated into medicinal extract, is cooled to 4 DEG C of preservations stand-by;
Folium cortex eucommiae the water extracted immersing paste: put into extractor after being pulverized by folium cortex eucommiae, add the water of 3 times of weight wherein, add hot reflux 2h, add a small amount of ethanol, after alcohol precipitation, filters, filtrate is concentrated into medicinal extract, is cooled to 4 DEG C of preservations stand-by;
Amargosa alcohol-extracted extract: put into extractor after being pulverized by amargosa, add 50% ethanol of 3 times of weight wherein, add hot reflux 2h, filter, filtrate is concentrated into medicinal extract, is cooled to 4 DEG C of preservations stand-by.
4. a preparation method for the emulsion for killing aphid and two spotted spider mite according to any one of claims 1 to 3, is characterized in that, comprise the following steps:
(1) tree-of-heaven leaf the water extracted immersing paste, kuh-seng alcohol-extracted extract, folium cortex eucommiae the water extracted immersing paste, amargosa alcohol-extracted extract are mixed in proportion, add solvent, in 30 ~ 50 DEG C of heating for dissolving, obtain liquid;
(2) in the liquid obtained, add emulsifier and auxiliary agent, utilize ultrasonic emulsification device, supersonic frequency is 10 ~ 15kHz, and ultrasonic time is 30 ~ 60min, and temperature is 50 ~ 70 DEG C, obtains primary emulsion;
(3) in primary emulsion, preservative, antifreezing agent and deionized water is slowly dripped successively, rate of addition is 2 ~ 5mL/min, in 40 ~ 60 DEG C of heating water baths, stir with 5000 ~ 8000r/min simultaneously, continue stirring 20 ~ 30min after dripping deionized water, stopping stirring, being slowly down to the faint yellow emulsion that namely room temperature obtains for killing aphid and two spotted spider mite, sealing, puts shady and cool place storage.
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| CN105325451A (en) * | 2015-11-27 | 2016-02-17 | 沧州大洋化工有限责任公司 | Insecticide composition and preparation method thereof |
| CN105409929B (en) * | 2015-11-27 | 2018-11-02 | 沧州大洋化工有限责任公司 | A kind of pesticide stabilizing synergistic agent and preparation method thereof |
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| CN102125061A (en) * | 2010-01-19 | 2011-07-20 | 北京联合大学生物化学工程学院 | Pesticide for killing aphid and red spider and preparation method thereof |
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