CN103814964A - Emulsion for killing aphid and red spider and its preparation method - Google Patents
Emulsion for killing aphid and red spider and its preparation method Download PDFInfo
- Publication number
- CN103814964A CN103814964A CN201410054908.0A CN201410054908A CN103814964A CN 103814964 A CN103814964 A CN 103814964A CN 201410054908 A CN201410054908 A CN 201410054908A CN 103814964 A CN103814964 A CN 103814964A
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- emulsion
- aphid
- add
- killing
- spider mite
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Abstract
The invention discloses emulsion for killing aphid and red spider and its preparation method. The emulsion uses mixed extractum as a main medicine, the mixed extractum comprises ailanthus altissima leaf water extraction extractum, radix sophorae flavescentis alcohol extraction extractum, eucommia ulmoides leaf water extraction extractum and neem bark alcohol extraction extractum with a weight ratio of 1:1:2:2, the emulsion also comprises, in relative to each gram of the main medicine, the following components: 40-50mL of a solvent, 5-15mL of an emulsifier, 0.05-0.15g of an assistant, 1-2mL of a preservative, 5-7.5mL of an antifreeze and 50-100mL of deionized water. The preparation method of the emulsion is as follows: (1) mixing the four extraction extractum according to the ratio, adding the solvent, heating for dissolving to obtain a medicine liquid; (2) adding the emulsifier and the assistant to the medicine liquid, using an ultrasonic emulsification device to obtain primary emulsion; (3) successively adding the preservative, the antifreeze and the deionized water to the primary emulsion, stirring, cooling to room temperature to obtain the emulsion. The emulsion is environmental friendly, stable in quality and good in insecticidal effect, and the preparation method has the advantages of simple operation and ow production cost.
Description
Technical field
The present invention relates to a kind ofly for killing emulsion of aphid and two spotted spider mite and preparation method thereof, belong 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 insect pest 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.What wherein more than 95% use is chemical pesticide, and biopesticide proportion is only 2%～3%, and emulsion is very few especially.Damage by disease and insect is being killed, suppressed to agricultural chemicals on the one hand, guarantees to play a very important role in crops high and stable yields, meanwhile, thereby also can jeopardize by all means due to irrational use the safety of environment, and then infringement health.China's height is malicious, highly toxic pesticide kind is in the majority, environment has been caused to extremely serious pollution, agricultural chemicals residual quantity in food agricultural produce exceeds the corresponding standard of country on a large scale, and have the trend that continues increase, the physical and mental health on the common people and export of farm produce trade formed serious infringement and impact.
Plant resource, microbial pesticide proportion in biogenic substances agricultural chemicals are relatively larger, are the important first stems of novel pesticide initiative.By the developmental research to plant resources, the floristics that discovery can become agricultural chemicals is a lot, mainly concentrates on the sections more than 30 such as Meliaceae, composite family, pulse family, Celastraceae, Euphorbiaceae for many years.The active substance relating 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, the biopesticide of effective, the non-environmental-pollution of preparation pest control, noresidue is significant.
People have done large quantity research for insecticide emulsion.The people such as Miao Kang, Shu Zhaolin studies by the control efficiency of 25% first dimension chlorpyrifos aqueous emulsion to wheat aphid, adopt emamectin-benzoate 0.2%, chlopyrifos 24.8%, built agent is controlled wheat aphid and is all played an important role in Wheat Production, and field trial shows: 25% first dimension chlorpyrifos aqueous emulsion control wheat aphid has advantages of 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 agricultural science, 2010,6:199-200) to the control efficiency of wheat aphid.The people such as Qin Guicong, Cen Liujun adopts and 4%, kills precious aqueous emulsion more 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 insect population decline rate of aphid has improved 2.27% (Guangxi Agricultural science, 2007,3:167-168).The people such as Cheng Hongsen study the control test of different miticides to Chinese rose of cut flower two spotted spider mite, find that 1500 times of dilutions of propargite are a kind of desirable medicaments (Agriculture of Anhui science, 2008,36:10536-10537) of preventing and treating two spotted spider mite.The people such as Sun Meimei, Chai Weigang studies 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: 2 kinds of extracts of garlic and tea seed cake have certain control effect 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 the optimization of total alkaloid from sophora flavescens ait extraction process and killing aphids activity research, by shrubby sophora extract, the insecticidal activity assay test of aphid is shown, Radix Sophorae Flavescentis extractive liquid is carried out to different disposal and with its insecticidal activity significant difference of different solvents; Take chloroform as extracting solvent, gained total alkaloid from sophora flavescens ait content is the highest, and its insecticidal activity is the highest; Take ethanol as extracting solvent, chloroform extract is compared with concentrate, in the time of same concentrations total alkaloids, chloroform extract is higher to aphid insecticidal activity, may be that in ethanol concentrate, impurities is more, total alkaloids insecticidal activity is caused to interference (Chinese Wild plant resources, 2008,27 (1): 43-46).
Patent documentation CN102578164A discloses a kind of plant resource compound synergic insecticide containing matrine and Macleaya cordata alkaloids and preparation method thereof, this plant resource synergistic complex insecticide making is main component by matrine and Macleaya cordata alkaloids and adds additive compound to form, and preparation form is environment-friendly type missible oil, aqua or soluble liquid; In preparation, contain matrine 0.1%～20%, Macleaya cordata alkaloids 0.1%～20%, all the other are auxiliary agent.Be mainly used in the pest such as control melon, aphid really, on vegetables, two spotted spider mite, fragrant-flowered garlic maggot, Paratrioza sinica, pear sucker, cabbage caterpillar, diamond-back moth, mythimna separata.Patent documentation CN102524271A discloses sparteine matrine disinsection aqueous emulsion, this sparteine matrine disinsection aqueous emulsion be by sparteine extract and the composite aqueous emulsion forming of matrine extract wherein the consumption of sparteine extract be 15%～20%, 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 in percent by volume.This invention mixes sparteine and matrine two Plants source alkaloids, thereby obtains efficient, low toxicity and the little biopesticide of environmental pollution.This invention main component such as sparteine and matrine used is all the natural products extracting from plant, and sparteine and matrine have insecticidal action, therefore insect are had to very strong killing action.Patent documentation CN101843262A discloses a kind of agricultural chemicals of preventing and treating 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, solvent is pulverized, added to castor seeds, dipping extracts and repeatedly merges afterwards extract, hydraulic pressure be concentrated into solvent evaporates after complete castor oil mother liquor, in castor oil mother liquor, add dissolution with solvents again, after add emulsifier, bleeding agent and antifreeze, after mixing, obtain castor oil emulsion finished product.This invention processing technology is simple, with low cost, and quick-acting is good, the lasting period is long, can significantly reduce access times and the using dosage of chemical pesticide, effectively reduces the persticide residue in melon dish, preserves the ecological environment, and promotes agricultural product quality and safety.
Patent documentation CN102125061A is disclosed a kind of for killing agricultural chemicals of aphid and two spotted spider mite and preparation method thereof, and 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 effective component extracting from tree-of-heaven leaf, folium cortex eucommiae and kuh-seng first, 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 effect is lasting, production cost is 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 for killing the new emulsion of aphid and two spotted spider mite, this emulsion environmental friendliness, steady quality, good disinsection effect.
The preparation method who another object of the present invention is to provide 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, the mixing medicinal extract that this emulsion forms take 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 main ingredient, and in main ingredient, the weight ratio of four kinds of medicinal extract is 1: 1: 2: 2.
In described emulsion, also comprise the component of following consumption with respect 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.
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 containing the ethylene glycol of 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 tree-of-heaven leaf is pulverized, add wherein the water of 4 times of weight, add hot reflux 2h, add a small amount of ethanol, after alcohol precipitation, filter, filtrate is concentrated into medicinal extract, be cooled to 4 ℃ of preservations stand-by;
Kuh-seng alcohol-extracted extract: kuh-seng is put into extractor, add wherein 50% ethanol of 4 times of weight, add hot reflux 2h, filter, filtrate is concentrated into medicinal extract, is cooled to 4 ℃ of preservations stand-by;
Folium cortex eucommiae the water extracted immersing paste: put into extractor after folium cortex eucommiae is pulverized, add wherein the water of 3 times of weight, add hot reflux 2h, add a small amount of ethanol, after alcohol precipitation, filter, filtrate is concentrated into medicinal extract, be cooled to 4 ℃ of preservations stand-by;
Amargosa alcohol-extracted extract: put into extractor after amargosa is pulverized, add wherein 50% ethanol of 3 times of weight, add hot reflux 2h, filter, filtrate is concentrated into medicinal extract, is cooled to 4 ℃ of preservations stand-by.
Described for killing the preparation method of emulsion for aphid and two spotted spider mite, 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 ℃ of heating for dissolving, obtain liquid;
(2) in the liquid obtaining, 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 ℃, obtains primary emulsion;
(3) in primary emulsion, slowly drip successively preservative, antifreezing agent and deionized water, rate of addition is 2～5mL/min, in 40～60 ℃ of heating water baths, stir with 5000～8000r/min simultaneously, after dripping deionized water, continue to stir 20～30min, stop stirring, be slowly down to room temperature and obtain the faint yellow emulsion 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, is then prepared into aqueous emulsion.The present invention uses a small amount of organic solvent, and take water as continuous phase, Liquid Insecticides is disperse phase, can suppress the volatilization of insecticide, avoids or has reduced toxicity and the excitant of organic solvent to people and animals.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 that deinsectization effect is lasting, 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.
It is raw material that the present invention adopts tree-of-heaven leaf, folium cortex eucommiae, amargosa and kuh-seng, and wherein tree-of-heaven has another name called Ailanthus altissima or wood rice huller tree, the ancient tree of heaven that claims.Having item wood, is Simarubaceae deciduous tree plant.Dispersing stink because of leaf base gland point gains the name.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, and widely distributed in China.Tree-of-heaven is the strongest to tobacco mosaic virus inhibitory action, and to cucumber mosaic virus, it is active that marmor upsilon has significant external inhibition, and having exploitation becomes the potentiality of plant antiviral agent.Form: deciduous tree, 30 meters of Gao Keda, tree crown is oblate spheroid or umbrella shape.Bark canescence or grey black, level and smooth, slightly checking.Sprig is sturdy.Leaf scar is large, obovate, 9 bundle scars of interior tool.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 ellipse, seed majority, has flat membranous wing.
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 filaments.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; Blade ellipse, avette or Long Circle, long 6-15cm, wide 3.5-6.5cm, tip is point gradually, the circular or wealthy wedge shape of base portion, above dirty-green, below pale green, Lao Ye is wrinkle slightly, 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 Room 1, tip 2 splits, and ovary handle is extremely short.Samara is flat, oblong, and tip 2 splits, base portion wedge shape, the around thin wing of tool; Nut is positioned at central authorities, has joint with carpopodium joint.Bloom early spring, after autumn fruit maturation.
Kuh-seng is called matrine, chuanshentong, phoenix claw, Niu Can etc., derives from the root of leguminous plant kuh-seng, and all produce all parts of the country, 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, and remove root head and little supporting root, cleaning, drying, or take advantage of fresh slices, dry.Proterties: this product is elongated cylindrical, branch is often arranged at bottom, long 10～30cm, diameter 1～2cm.Surface taupe brown or brown color, the vertical wrinkle of tool and the hole skin of growing crosswise.Crust is thin, and the warp that breaks, easily peels off more, 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 having.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 skins.Two to three times imparipinnate leaf alternates, are born in wilderness or roadside, often cultivate after room anterior chamber.Distribute north to Hebei, reach Guangxi, Yunnan in the south, to Sichuan and other places.In chinaberry bark, contain toosendanin (toosendanin), China tree ketone (kulinone), China tree terpene ketone lactone (kulactone), China tree terpene alcoholic lactone.Nature and flavor: hardship; Cold; Poisonous.Function cures mainly: have ascarifuge, in pinworm and whip.As a kind of separation from the branch skin of Meliaceae and China tree and come plant insecticide, there is stomach toxicity, tag and certain Antifeedant Effects.
Tree-of-heaven leaf used in the present invention is plucked the garden with hundreds of grasses in Biochemical Engineering College of Beijing Union University, plucking time is annual summer, folium cortex eucommiae is plucked the Practical Teaching Base in Anguo Biochemical Engineering College of Beijing Union University, Hebei, plucking time is annual summer, dry kuh-seng and be purchased from Xuancheng Bai Cao Co., Ltd, 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 tree-of-heaven leaf is pulverized, add wherein the water of 4 times of weight, add hot reflux 2h, add a small amount of ethanol, after alcohol precipitation, filter, filtrate is concentrated into medicinal extract, be cooled to 4 ℃ of preservations stand-by;
Kuh-seng alcohol-extracted extract: kuh-seng is put into extractor, add wherein 50% ethanol of 4 times of weight, add hot reflux 2h, filter, filtrate is concentrated into medicinal extract, is cooled to 4 ℃ of preservations stand-by;
Folium cortex eucommiae the water extracted immersing paste: put into extractor after folium cortex eucommiae is pulverized, add wherein the water of 3 times of weight, add hot reflux 2h, add a small amount of ethanol, after alcohol precipitation, filter, filtrate is concentrated into medicinal extract, be cooled to 4 ℃ of preservations stand-by;
Amargosa alcohol-extracted extract: put into extractor after amargosa is pulverized, add wherein 50% ethanol of 3 times of weight, add hot reflux 2h, filter, filtrate is concentrated into medicinal extract, is cooled to 4 ℃ of preservations stand-by.
Embodiment 1
By 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 according to weight ratio 1: 1: 2: 2 are mixed to get 2.0g mixing medicinal extract, add in n-hexane (or dimethylbenzene, cyclohexanone, cyclohexanol, 200# solvent naphtha), in 40 ℃ of heating for dissolving, obtain liquid; Amount according to prescription 1 joins emulsifier tween 80 and auxiliary agent sodium carboxymethylcellulose in the liquid of configuration, utilizes ultrasonic emulsification device, and supersonic frequency is 15kHz, and ultrasonic time is that 30min, temperature are 60 ℃, obtains primary emulsion; In primary emulsion, slowly drip the ethylparaben of 5%g/mL, ethylene glycol solution and the deionized water of 5%g/mL, rate of addition is 3mL/min, in 60 ℃ of heating water baths, stir with 7000r/min simultaneously, after dripping deionized water, continue to stir 30min, after emulsion forms, answer slow cooling, when cooling, should not stir, to prevent drop gathering, obtain killing the faint yellow emulsion of 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 do not have layering |
| Dimethylbenzene | 178.52±59.37 | Long-term placement do not have layering |
| Cyclohexanone | 197.28±93.57 | Place and within 60 days, have lamination |
| Cyclohexanol | 194.32±47.39 | Place and within 37 days, have lamination |
| 200# solvent naphtha | 204.18±68.39 | Place and within 40 days, have lamination |
Embodiment 2
By 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 according to weight ratio 1: 1: 2: 2 are mixed to get 2.0g mixing medicinal extract, add in n-hexane solvent, in 40 ℃ of heating for dissolving, obtain liquid; Amount according to prescription 2 joins emulsifier tween 60 (or Tween 80) and auxiliary agent sodium carboxymethylcellulose in the liquid of configuration, utilize ultrasonic emulsification device, supersonic frequency is 15kHz, and ultrasonic time is that 30min, temperature are 60 ℃, obtains primary emulsion; In primary emulsion, slowly drip the ethylparaben of 5%g/mL, ethylene glycol solution and the deionized water of 5%g/mL, rate of addition is 3mL/min, in 60 ℃ of heating water baths, stir with 7000r/min simultaneously, after dripping deionized water, continue to stir 30min, after emulsion forms, answer slow cooling, when cooling, should not stir, to prevent drop gathering, obtain killing the faint yellow emulsion of 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 ℃.Precision measures emulsion 50 μ L in 50mL measuring bottle, is diluted to scale with pure water, gets appropriate solution and measure in sample cell the zeta current potential of emulsion.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 |
In prescription, adopt emulsifier tween 80, zeta current potential absolute value is larger, and its interparticle electrostatic repulsion is also just larger, and physical stability is also just better.In order to observe at short notice the layering of emulsion, adopt centrifugal process 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 continuously the efficiency test in three seasons, each season, parallel doing three times, investigated agricultural-chemical emulsion of the present invention (I), dichlorvos (II) and the control efficiency of flolimat (III) to aphid, two spotted spider mite.Experimental result is as shown in Table 3, 4:
The control efficiency of table 33 kind of insecticide to aphid
The control efficiency of table 43 kind of insecticide to two spotted spider mite
Wherein:
Test shows: agricultural-chemical emulsion of the present invention was all better than chemical pesticide since the 3rd day to the preventive effect of aphid, two spotted spider mite; By the 7th day, the correction preventive effect of aphid is still greater than to 80%, the correction preventive effect of two spotted spider mite is greater than to 75%, lasting effect is better; Test is shown to: this pesticide price is only 1.43 times of dichlorvos price 1.37 times of flolimat by the cost accounting data of agricultural chemicals.
Embodiment 4
By 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 according to weight ratio 1: 1: 2: 2 are mixed to get 2.0g mixing medicinal extract, add in n-hexane solvent, in 40 ℃ of heating for dissolving, obtain liquid; Amount according to prescription 3 joins emulsifier tween 80 and auxiliary agent sodium carboxymethylcellulose in the liquid of configuration, utilizes ultrasonic emulsification device, and supersonic frequency is 15kHz, and ultrasonic time is that 30min, temperature are 60 ℃, obtains primary emulsion; Slowly drip the ethylparaben of 5%g/mL, ethylene glycol solution and the deionized water of 5%g/mL to colostrum, rate of addition is 3mL/min, in 60 ℃ of heating water baths, stir with 7000r/min simultaneously, after dripping deionized water, continue to stir 30min, after emulsion forms, answer slow cooling, when cooling, should not stir, to prevent drop gathering, obtain killing the faint yellow emulsion of 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 is write standard ", 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, standard hard water dilution for microemulsion sample, 30 ℃ of constant volumes in volumetric flask, leave standstill 1h, observe during this period microemulsion emulsion-stabilizing situation, as separated out without crystallization or oil slick, the oil that sinks, also there is not suspension or become muddy, think that stability of emulsion is qualified.
2, low-temperature stability test
Undertaken by GB/T19137-2003, take out, return to room temperature, through slowly shake, separate out as qualified without visible solid particle or grease.
3, heat storage stability test
Undertaken by GB/T19136-2003.Gainer is tested, and its result still meets standard-required, is qualified.
4, pourability test
The sample that is placed in container is placed after certain hour, and program is toppled over according to the rules, measures the amount that is trapped in sample in container, after container is washed with water, then measures the sample size in container, and this agricultural-chemical emulsion does target with matrine content.
Table 5 emulsion quality and technical index
Claims (9)
1. one kind for killing the emulsion of aphid and two spotted spider mite, it is characterized in that, the mixing medicinal extract that this emulsion forms take 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 main ingredient, and in main ingredient, the weight ratio of four kinds of medicinal extract is 1: 1: 2: 2.
2. according to claim 1 for killing the emulsion of aphid and two spotted spider mite, it is characterized in that, in described emulsion, also comprise the component of following consumption with respect 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.
3. according to claim 1 and 2ly it is characterized in that for killing the emulsion of aphid and two spotted spider mite, described solvent is n-hexane, dimethylbenzene, cyclohexanone, cyclohexanol or 200# solvent naphtha.
4. according to claim 1 and 2ly it is characterized in that for killing the emulsion of aphid and two spotted spider mite, described emulsifier is polysorbas20, polysorbate60, polysorbate65, Tween 80 or polysorbate85.
5. according to claim 1 and 2ly it is characterized in that for killing the emulsion of aphid and two spotted spider mite, described auxiliary agent is sodium carboxymethylcellulose.
6. according to claim 1 and 2ly it is characterized in that for killing the emulsion of aphid and two spotted spider mite, described preservative is the ethanolic solution of 5%g/mL ethylparaben.
7. according to claim 1 and 2ly it is characterized in that the aqueous solution of the ethylene glycol that described antifreezing agent is 5%g/mL for killing the emulsion of aphid and two spotted spider mite.
8. according to claim 1ly it is characterized in that for killing the emulsion of aphid and two spotted spider mite, the preparation method of described four kinds of medicinal extract is:
Tree-of-heaven leaf the water extracted immersing paste: put into extractor after tree-of-heaven leaf is pulverized, add wherein the water of 4 times of weight, add hot reflux 2h, add a small amount of ethanol, after alcohol precipitation, filter, filtrate is concentrated into medicinal extract, be cooled to 4 ℃ of preservations stand-by;
Kuh-seng alcohol-extracted extract: kuh-seng is put into extractor, add wherein 50% ethanol of 4 times of weight, add hot reflux 2h, filter, filtrate is concentrated into medicinal extract, is cooled to 4 ℃ of preservations stand-by;
Folium cortex eucommiae the water extracted immersing paste: put into extractor after folium cortex eucommiae is pulverized, add wherein the water of 3 times of weight, add hot reflux 2h, add a small amount of ethanol, after alcohol precipitation, filter, filtrate is concentrated into medicinal extract, be cooled to 4 ℃ of preservations stand-by;
Amargosa alcohol-extracted extract: put into extractor after amargosa is pulverized, add wherein 50% ethanol of 3 times of weight, add hot reflux 2h, filter, filtrate is concentrated into medicinal extract, is cooled to 4 ℃ of preservations stand-by.
In claim 1 to 8 described in any one for killing the preparation method of emulsion for aphid and two spotted spider mite, it 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 ℃ of heating for dissolving, obtain liquid;
(2) in the liquid obtaining, 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 ℃, obtains primary emulsion;
(3) in primary emulsion, slowly drip successively preservative, antifreezing agent and deionized water, rate of addition is 2～5mL/min, in 40～60 ℃ of heating water baths, stir with 5000～8000r/min simultaneously, after dripping deionized water, continue to stir 20～30min, stop stirring, be slowly down to room temperature and obtain the faint yellow emulsion for killing aphid and two spotted spider mite, sealing, puts shady and cool place storage.
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| CN108077329A (en) * | 2017-12-05 | 2018-05-29 | 大新县科学技术情报研究所 | A kind of lemon nutritive insecticidal injection drying agent and preparation method thereof |
| CN109430305A (en) * | 2018-11-29 | 2019-03-08 | 淳安县蚕桑管理总站 | It is a kind of for the insecticide and its preparation process of diaphania and application |
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