CN103651588A - Preparation method for microcapsule pesticide for killing aphids - Google Patents
Preparation method for microcapsule pesticide for killing aphids Download PDFInfo
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- CN103651588A CN103651588A CN201310409373.XA CN201310409373A CN103651588A CN 103651588 A CN103651588 A CN 103651588A CN 201310409373 A CN201310409373 A CN 201310409373A CN 103651588 A CN103651588 A CN 103651588A
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Abstract
The invention discloses a preparation method for a microcapsule pesticide for killing aphids. The preparation method comprises the following steps of (1) smashing ailanthus leaves, putting the smashed ailanthus leaves into an extracting pot, adding water into the extracting pot, performing heating backflow for 2 hours, filtering and concentrating the solution until the amount of the solution is 10 percent of the total amount of medicinal liquid to obtain an ailanthus leaf extract concentrated solution; (2) putting cigarette ends into an ultrasonic extracting pot, adding the water and a 10% hydrochloric acid solution for immersion for 30-40min, performing ultrasonic extraction at the temperature of 20-50 DEG C and the frequency of 20 kHz for 20-60min, performing filtration, adding 30-50% NaOH into filtrate, stirring the filtrate and the NaOH until the solution is obviously in an alkaline state, and distilling the alkaline solution through water vapor to obtain nicotine; and (3) adding the nicotine, PEG (polyethylene glyco), Span and cholesterol into dichloromethane for stirring and dissolving, performing rotary evaporation in a constant-temperature water bath with the temperature of 40 DEG C to remove an organic solvent, forming a uniform film on a bottle wall, vacuumizing and staying for one night, injecting the ailanthus leaf extract concentrated solution into the materials during continuous stirring, performing hydration at the temperature of 70 DEG C for 30min, and performing ultrasonic emulsification for 8-13 hours to obtain the semi-transparent microcapsule pesticide. The method is low in production cost, and the technology is easy to operate; the prepared microcapsule pesticide has a lasting effect on deinsectization and a good effect of preventing and treating insect pests, is pollution-free to the environment and cannot be retained.
Description
Technical field
The present invention relates to a kind ofly for killing the preparation method of the encapsulate pesticides of aphid, belong to natural plants applied technical field.
Background technology
Plant resource in biogenic substances agricultural chemicals, microbial pesticide proportion are relatively large, 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 Meliaceae, composite family, pulse family, Celastraceae, Euphorbiaceae Deng30Duo section for many years.The active substance relating generally to is: glucosides class (as gleditsin Aglycone, crotons glucosides, tomatin), phenols and quinones (as gossypol, Walnut Leaves quinone and shrubby flase indigo element), alkaloids (as nicotine, wilfordine), terpene (as firpene, live that happy wood is normal, toosendanin and nimbin), steroid class (as ponasterone and Inokosterone).Therefore, preparation pest control is effective, non-environmental-pollution, and the biopesticide of noresidue is significant.
Patent documentation CN102246835A discloses Compositional phytochemicals pesticide, its technical scheme main points are: margosine, matrine, tree-of-heaven juice, datura flower are pressed to column weight amount than formulated, 0.2～0.5 part of margosine, 0.3～0.5 part of matrine, 5～50 parts, tree-of-heaven juice, 0.1～0.5 part of datura flower, also can add appropriate water, can prevent and treat cabbage caterpillar, diamond-back moth, Oeobia undalis, aphid, prodenia litura, tealeaves caterpillar, dish ant, rice fulgorid, rice volume snout moth's larva, borer etc.
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, composition of raw materials 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.
Patent documentation CN101926372A discloses a kind of nicotine matrine agent plant pesticide and preparation method thereof, this invention insecticide specially kills Unaspis yanonensis, and can kill cottonycushion scale, chaff scale, brown round a red-spotted lizard, ceroplastes rubens, blister mite, two spotted spider mite, four spot yellow spiders, leaf miner, aphid etc.
Summary of the invention
The object of the present invention is to provide that a kind of prepared encapsulate pesticides is used for killing aphid for killing the preparation method of the encapsulate pesticides of aphid, environmental protection is useful and harmless to environment.
For achieving the above object, the present invention is by the following technical solutions:
For killing a preparation method for the encapsulate pesticides of aphid, comprise the following steps:
1) tree-of-heaven leaf is pulverized, put into extractor, add wherein water, the mass ratio of tree-of-heaven leaf and water is 1: 4, adds hot reflux 2h, filters, and is concentrated into 10% of total amount of liquid medicine and obtains tree-of-heaven leaf extraction concentrate;
2) cigarette end is put into ultrasonic extraction tank, add water and 10% hydrochloric acid solution to soak 30～40min, wherein the mass ratio between cigarette end, water and hydrochloric acid solution is 1: 4: 1, in ultrasonic extraction 20～60min of 20～50 ℃ of proportion 20kHz, filter, to adding concentration in filtrate, be 30～50%NaOH, be stirred to and be obvious alkalescence, mixed liquor is obtained to water white oily liquid through steam distillation, be nicotine, be cooled to 4 ℃ of preservations stand-by;
3) nicotine, PEG, sapn and cholesterol are added to stirring and dissolving in organic solvent dichloromethane, in 40 ℃ of waters bath with thermostatic control, rotary evaporation is except organic solvent, on bottle wall, form homogeneous film, vacuumize and spend the night, in constantly stirring, inject tree-of-heaven leaf and extract concentrate, in 70 ℃ of aquation 30min, ultrasonic emulsification 8～13h, obtains translucent encapsulate pesticides.
In the preparation process of encapsulate pesticides, PEG, sapn are as surfactant, and cholesterol has the effect that regulates membrane fluidity, nicotine, PEG, sapn and cholesterol are dissolved in organic solvent dichloromethane, utilize film dispersion-ultrasonic method to prepare encapsulate pesticides.
Described step 1) in, tree-of-heaven leaf is crushed to 24 orders.
The molecular weight of described PEG is 4000 or 6000.
Described sapn is span 20 or sorbester p18.
Mass ratio between described nicotine, PEG, sapn, cholesterol is (0.5～1): 5: 2: 1.
Described step 3) mass ratio that the tree-of-heaven leaf adding in extracts between concentrate and nicotine is 1: (1～3).
The invention has the advantages that:
The present invention utilizes the active ingredient in solvent extraction plant tree-of-heaven leaf, and adopt ultrasonic method to extract the nicotine in discarded object cigarette end, utilize film dispersion-aquation ultrasonic method to be prepared into microcapsule formulation, avoid or reduced organic solvent to people and animals' toxicity and excitant, micro-capsule steady quality, effective drug duration is long, kills the liquid preparation that aphid effect is better than the chemical pesticides such as dichlorvos and flolimat and formulation of pesticide in 15 days.
Production cost of the present invention is low, technological operation is simple, and test is shown with the cost accounting data of agricultural chemicals: adopting pesticide price prepared by the present invention is only 1.52 times of dichlorvos price, 1.61 times of flolimat.
The encapsulate pesticides deinsectization effect that adopts the present invention to make is lasting, pest control is effective, non-environmental-pollution, and noresidue, is a kind of natural green agricultural chemicals of environment-friendly type.
Accompanying drawing explanation
Fig. 1 is the influence curve figure of phaco time to microencapsulation rate in embodiment 2.
Embodiment
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, and plucking time is annual summer, and cigarette end is collected in each office of school.
Embodiment 1
2.5kg tree-of-heaven leaf is pulverized, put into extractor, add wherein 10L water, add hot reflux 2h, be concentrated into 10% of total amount of liquid medicine and obtain tree-of-heaven leaf extraction concentrate, be cooled to 4 ℃ of preservations stand-by; By 2.0kg cigarette end, put into ultrasonic extraction tank, add 8L water and 10% hydrochloric acid solution 2L to soak 30min, proportion 20kHz's is ultrasonic, and 40 ℃ of extraction 30min of temperature, filter, in filtrate, adding concentration is 40%NaOH, is stirred to and is obvious alkalescence (checking with litmus red test paper).Steam distillation device is installed, mixed liquor is poured in round-bottomed flask with long neck, carry out steam distillation, collect and obtain water white oily liquid nicotine, be cooled to 4 ℃ of preservations stand-by.
Take 0.1g nicotine, 0.5gPEG, 0.2g sapn and 0.1g cholesterol and add stirring and dissolving in 50mL organic solvent dichloromethane, in 40 ℃ of waters bath with thermostatic control, rotary evaporation is except organic solvent, make filmogen form homogeneous film at bottle wall, putting into 60 ℃ of vacuum drying chambers vacuumizes and spends the night, in constantly stirring, inject tree-of-heaven leaf and extract concentrate 50mg, in 70 ℃ of aquation 30min, ultrasonic emulsification 10h, obtains translucent encapsulate pesticides.With ultraviolet-uisible spectrophotometer, quantitatively detect the content of nicotine, envelop rate %=W
bag/ W
always, different PEG, sapn are on forming the impact of micro-capsule, and in 40 times of electron microscopes, observed result is as shown in table 1.
The different PEG of table 1, sapn are on forming the impact of micro-capsule
| Capsule material component | Micro-capsule outward appearance | Envelop rate % |
| PEG600, sorbester p18 | Capsule material has many not dissolvings | - |
| PEG1000, sorbester p18 | Particle size is inhomogeneous | 48.7 |
| PEG4000, sorbester p18 | Microcapsule diameter is uniformly distributed | 57.2 |
| PEG6000, sorbester p18 | Microcapsule diameter is uniformly distributed | 76.3 |
| PEG6000, |
Microcapsule diameter is uniformly distributed | 60.5 |
Embodiment 2
2.5kg tree-of-heaven leaf is pulverized, put into extractor, add wherein 10L water, add hot reflux 2h, be concentrated into 10% of total amount of liquid medicine and obtain tree-of-heaven leaf extraction concentrate, be cooled to 4 ℃ of preservations stand-by; By 2.0kg cigarette end, put into ultrasonic extraction tank, add 8L water and 10% hydrochloric acid solution 2L to soak 30min, proportion 20kHz's is ultrasonic, and 40 ℃ of extraction 30min of temperature, filter, in filtrate, add 40%NaOH, be stirred to and be obvious alkalescence (checking with litmus red test paper).Reduced pressure concentration steams water and obtains nicotine, is cooled to 4 ℃ of preservations stand-by.
Take 0.1g nicotine, 0.5gPEG6000,0.2g sorbester p18 and 0.1g cholesterol and add stirring and dissolving in 50mL organic solvent dichloromethane, in 40 ℃ of waters bath with thermostatic control, rotary evaporation is except organic solvent, make filmogen form homogeneous film at bottle wall, putting into 60 ℃ of vacuum drying chambers vacuumizes and spends the night, in constantly stirring, inject tree-of-heaven leaf and extract concentrate 50mg, in 70 ℃ of aquation 30min, ultrasonic emulsification 8～13h, obtains translucent encapsulate pesticides.Phaco time on the impact of microencapsulation rate as shown in Figure 1.
In the ultrasonic time scope of 10～12h, the envelop rate of liposome is higher.Overlong time can be destroyed the structure of micro-capsule, the nicotine of sealing is revealed, thereby reduced envelop rate.And the time is too short, though envelop rate is large, system is uniform and stable not.During ultrasonic 10h left and right, the resultant effects such as envelop rate, particle diameter are better.
Embodiment 3
2.5kg tree-of-heaven leaf is pulverized, put into extractor, add wherein 10L water, add hot reflux 2h, be concentrated into 10% of total amount of liquid medicine and obtain tree-of-heaven leaf extraction concentrate, be cooled to 4 ℃ of preservations stand-by; By 2.0kg cigarette end, put into ultrasonic extraction tank, add 8L water, 10% hydrochloric acid solution 2L soaks 30min, and proportion 20kHz's is ultrasonic, 40 ℃ of extraction 30min of temperature, filter, in filtrate, add 40%NaOH, be stirred to and be obvious alkalescence (checking with litmus red test paper).Reduced pressure concentration steams water and obtains nicotine, is cooled to 4 ℃ of preservations stand-by.
Take 0.1g nicotine, 0.5gPEG6000,0.2g sorbester p18 and 0.1g cholesterol and add stirring and dissolving in 50mL organic solvent dichloromethane, in 40 ℃ of waters bath with thermostatic control, rotary evaporation is except organic solvent, make filmogen form homogeneous film at bottle wall, putting into 60 ℃ of vacuum drying chambers vacuumizes and spends the night, in constantly stirring, inject tree-of-heaven leaf and extract concentrate 50mg, in 70 ℃ of aquation 30min, ultrasonic emulsification 10h, obtains translucent encapsulate pesticides.
Utilize agricultural chemicals and the conventional chemical pesticide efficiency test that method of the present invention obtains to contrast:
I: tree-of-heaven leaf nicotinic liquid body preparation: tree-of-heaven leaf extract: nicotine=5: 1 (mass ratio);
II: tree-of-heaven leaf nicotine microcapsule formulation;
III: get in 75% DDT EC 1mL to 2000mL tun, adding distil water is diluted to 1500mL;
IV: get in 48% omethoate emulsifiable solution 1mL to 2000mL tun, adding distil water is diluted to 1500mL;
V: clear water.
Do continuously the efficiency test in three seasons, each season, parallel doing three times, investigated agricultural chemicals of the present invention, dichlorvos and the flolimat control efficiency to aphid.Experimental result is as shown in table 2:
The control efficiency of 4 kinds of insecticides of table 2 to aphid
Wherein:
Test shows: encapsulate pesticides preparation of the present invention is suitable with chemical pesticide to the control efficiency to the of aphid 3 days; From the 7th day by the 15th day, the correction preventive effect of aphid is all greater than to 60%, is better than the control efficiency of chemical pesticide, lasting effect is better, compares also highly significant with the liquid preparation control efficiency of this agricultural chemicals.
Claims (7)
1. for killing a preparation method for the encapsulate pesticides of aphid, it is characterized in that, comprise the following steps:
1) tree-of-heaven leaf is pulverized, put into extractor, add wherein water, the mass ratio of tree-of-heaven leaf and water is 1: 4, adds hot reflux 2h, filters, and is concentrated into 10% of total amount of liquid medicine and obtains tree-of-heaven leaf extraction concentrate, is cooled to 4 ℃ of preservations stand-by;
2) cigarette end is put into ultrasonic extraction tank, add water and 10% hydrochloric acid solution to soak 30～40min, wherein the mass ratio between cigarette end, water and hydrochloric acid solution is 1: 4: 1, in ultrasonic extraction 20～60min of 20～50 ℃ of proportion 20kHz, filter, to adding concentration in filtrate, be 30～50%NaOH, be stirred to and be obvious alkalescence, mixed liquor is obtained to water white oily liquid through steam distillation, be nicotine, be cooled to 4 ℃ of preservations stand-by;
3) nicotine, PEG, sapn and cholesterol are added to stirring and dissolving in organic solvent dichloromethane, in 40 ℃ of waters bath with thermostatic control, rotary evaporation is except organic solvent, on bottle wall, form homogeneous film, vacuumize and spend the night, in constantly stirring, inject tree-of-heaven leaf and extract concentrate, in 70 ℃ of aquation 30min, ultrasonic emulsification 8～13h, obtains translucent encapsulate pesticides.
2. according to claim 1ly for killing the preparation method of the encapsulate pesticides of aphid, it is characterized in that described step 1) in tree-of-heaven leaf is crushed to 24 orders.
3. according to claim 1ly for killing the preparation method of the encapsulate pesticides of aphid, it is characterized in that, the molecular weight of described PEG is 4000 or 6000.
4. according to claim 1ly for killing the preparation method of the encapsulate pesticides of aphid, it is characterized in that, described sapn is span 20 or sorbester p18.
5. according to claim 1ly for killing the preparation method of the encapsulate pesticides of aphid, it is characterized in that, the mass ratio between described nicotine, PEG, sapn, cholesterol is (0.5～1): 5: 2: 1.
6. according to claim 1ly for killing the preparation method of the encapsulate pesticides of aphid, it is characterized in that described step 3) in the mass ratio that extracts between concentrate and nicotine of the tree-of-heaven leaf that adds be 1: (1～3).
7. according to claim 1ly for killing the preparation method of the encapsulate pesticides of aphid, it is characterized in that described step 3) in phaco time be 10h.
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Cited By (3)
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| CN106259557A (en) * | 2016-08-15 | 2017-01-04 | 卞佳林 | A kind of preparation method of flowering plum microencapsulation insecticide |
| CN106490023A (en) * | 2016-10-21 | 2017-03-15 | 赖丰光 | A kind of plant pesticide |
| CN113390810A (en) * | 2021-07-16 | 2021-09-14 | 中国烟草总公司四川省公司 | Nicotine extraction method and nicotine content determination method for fresh tobacco leaves |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106259557A (en) * | 2016-08-15 | 2017-01-04 | 卞佳林 | A kind of preparation method of flowering plum microencapsulation insecticide |
| CN106490023A (en) * | 2016-10-21 | 2017-03-15 | 赖丰光 | A kind of plant pesticide |
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