CN101390518A - Plant pesticide of micro-emulsion and its preparing method - Google Patents
Plant pesticide of micro-emulsion and its preparing method Download PDFInfo
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- CN101390518A CN101390518A CN 200710059741 CN200710059741A CN101390518A CN 101390518 A CN101390518 A CN 101390518A CN 200710059741 CN200710059741 CN 200710059741 CN 200710059741 A CN200710059741 A CN 200710059741A CN 101390518 A CN101390518 A CN 101390518A
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- 239000000575 pesticide Substances 0.000 title claims abstract description 43
- 239000004530 micro-emulsion Substances 0.000 title claims abstract description 13
- 238000000034 method Methods 0.000 title claims abstract description 5
- 239000008096 xylene Substances 0.000 claims abstract description 50
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims abstract description 49
- 241001671204 Stemona Species 0.000 claims abstract description 46
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 33
- SNICXCGAKADSCV-JTQLQIEISA-N (-)-Nicotine Chemical compound CN1CCC[C@H]1C1=CC=CN=C1 SNICXCGAKADSCV-JTQLQIEISA-N 0.000 claims abstract description 20
- 229960002715 nicotine Drugs 0.000 claims abstract description 20
- SNICXCGAKADSCV-UHFFFAOYSA-N nicotine Natural products CN1CCCC1C1=CC=CN=C1 SNICXCGAKADSCV-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000002904 solvent Substances 0.000 claims abstract description 15
- 238000002360 preparation method Methods 0.000 claims abstract description 11
- PAWQVTBBRAZDMG-UHFFFAOYSA-N 2-(3-bromo-2-fluorophenyl)acetic acid Chemical compound OC(=O)CC1=CC=CC(Br)=C1F PAWQVTBBRAZDMG-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000004254 Ammonium phosphate Substances 0.000 claims abstract description 10
- 229910000148 ammonium phosphate Inorganic materials 0.000 claims abstract description 10
- 235000019289 ammonium phosphates Nutrition 0.000 claims abstract description 10
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 65
- 239000002917 insecticide Substances 0.000 claims description 32
- 238000002386 leaching Methods 0.000 claims description 32
- 239000003795 chemical substances by application Substances 0.000 claims description 24
- 239000007788 liquid Substances 0.000 claims description 24
- 239000002585 base Substances 0.000 claims description 23
- 239000000203 mixture Substances 0.000 claims description 23
- 230000003389 potentiating effect Effects 0.000 claims description 23
- 238000000605 extraction Methods 0.000 claims description 16
- 238000003756 stirring Methods 0.000 claims description 14
- 239000004094 surface-active agent Substances 0.000 claims description 11
- 239000003513 alkali Substances 0.000 claims description 9
- 238000005660 chlorination reaction Methods 0.000 claims description 9
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 claims description 9
- POQHFALZNYMCBA-UHFFFAOYSA-N Stemonine Natural products CCC1C2C3CCC(C4CC(C)C(=O)O4)N3CCC(=O)C2OC15OC(=O)C(=C5)C POQHFALZNYMCBA-UHFFFAOYSA-N 0.000 claims description 8
- GYOGHROCTSEKDY-UHFFFAOYSA-N Tuberostemonine J Natural products C12N3CCCCC1C(CC)C1OC(=O)C(C)C1C2CC3C1CC(C)C(=O)O1 GYOGHROCTSEKDY-UHFFFAOYSA-N 0.000 claims description 8
- 230000006837 decompression Effects 0.000 claims description 8
- 235000012054 meals Nutrition 0.000 claims description 8
- 238000004064 recycling Methods 0.000 claims description 8
- 238000010992 reflux Methods 0.000 claims description 8
- 238000004062 sedimentation Methods 0.000 claims description 8
- UINUUSQOLRQGNF-UHFFFAOYSA-N stemonine Chemical compound O1C2(C=C(C)C(=O)O2)C(CC)C(C2CC3)C1CCCN2C3C1CC(C)C(=O)O1 UINUUSQOLRQGNF-UHFFFAOYSA-N 0.000 claims description 8
- HTLBMAZNGBFLEY-UHFFFAOYSA-N stemonine-C17 Natural products O1C(=O)C(C)CC1C1N2CCCC3OC(=O)C(C)C3C2CC1 HTLBMAZNGBFLEY-UHFFFAOYSA-N 0.000 claims description 8
- ZNQVEEAIQZEUHB-UHFFFAOYSA-N 2-ethoxyethanol Chemical compound CCOCCO ZNQVEEAIQZEUHB-UHFFFAOYSA-N 0.000 claims description 7
- REYJJPSVUYRZGE-UHFFFAOYSA-O hydron;octadecan-1-amine Chemical compound CCCCCCCCCCCCCCCCCC[NH3+] REYJJPSVUYRZGE-UHFFFAOYSA-O 0.000 claims description 6
- 239000002280 amphoteric surfactant Substances 0.000 claims description 5
- POAOYUHQDCAZBD-UHFFFAOYSA-N 2-butoxyethanol Chemical compound CCCCOCCO POAOYUHQDCAZBD-UHFFFAOYSA-N 0.000 claims description 4
- 239000003945 anionic surfactant Substances 0.000 claims description 3
- 238000009472 formulation Methods 0.000 claims description 3
- 235000013311 vegetables Nutrition 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 2
- KAATUXNTWXVJKI-NSHGMRRFSA-N (1R)-cis-(alphaS)-cypermethrin Chemical compound CC1(C)[C@@H](C=C(Cl)Cl)[C@H]1C(=O)O[C@H](C#N)C1=CC=CC(OC=2C=CC=CC=2)=C1 KAATUXNTWXVJKI-NSHGMRRFSA-N 0.000 abstract description 5
- 241000196324 Embryophyta Species 0.000 abstract description 5
- 238000003912 environmental pollution Methods 0.000 abstract description 3
- NYPJDWWKZLNGGM-UHFFFAOYSA-N fenvalerate Chemical compound C=1C=C(Cl)C=CC=1C(C(C)C)C(=O)OC(C#N)C(C=1)=CC=CC=1OC1=CC=CC=C1 NYPJDWWKZLNGGM-UHFFFAOYSA-N 0.000 abstract description 3
- 239000004480 active ingredient Substances 0.000 abstract description 2
- 239000003337 fertilizer Substances 0.000 abstract description 2
- 238000003860 storage Methods 0.000 abstract description 2
- 240000000233 Melia azedarach Species 0.000 abstract 2
- 239000003175 pesticide synergist Substances 0.000 abstract 2
- 238000012272 crop production Methods 0.000 abstract 1
- 230000001737 promoting effect Effects 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 24
- 238000004128 high performance liquid chromatography Methods 0.000 description 12
- 239000012141 concentrate Substances 0.000 description 6
- 239000000796 flavoring agent Substances 0.000 description 6
- 235000019634 flavors Nutrition 0.000 description 6
- 238000010298 pulverizing process Methods 0.000 description 6
- 238000002474 experimental method Methods 0.000 description 4
- 230000003449 preventive effect Effects 0.000 description 4
- ZSBXGIUJOOQZMP-UHFFFAOYSA-N Isomatrine Natural products C1CCC2CN3C(=O)CCCC3C3C2N1CCC3 ZSBXGIUJOOQZMP-UHFFFAOYSA-N 0.000 description 3
- ZSBXGIUJOOQZMP-JLNYLFASSA-N Matrine Chemical compound C1CC[C@H]2CN3C(=O)CCC[C@@H]3[C@@H]3[C@H]2N1CCC3 ZSBXGIUJOOQZMP-JLNYLFASSA-N 0.000 description 3
- -1 butyl glycol ethers Chemical class 0.000 description 3
- 239000003093 cationic surfactant Substances 0.000 description 3
- 239000003814 drug Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 229930014456 matrine Natural products 0.000 description 3
- UBGMVJFCVKEMNB-UHFFFAOYSA-N octadecan-3-amine Chemical compound CCCCCCCCCCCCCCCC(N)CC UBGMVJFCVKEMNB-UHFFFAOYSA-N 0.000 description 3
- 241000273311 Aphis spiraecola Species 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000006071 cream Substances 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 244000283070 Abies balsamea Species 0.000 description 1
- 235000007173 Abies balsamea Nutrition 0.000 description 1
- 241000553739 Aconitum carmichaelii var. truppelianum Species 0.000 description 1
- 235000001405 Artemisia annua Nutrition 0.000 description 1
- 240000000011 Artemisia annua Species 0.000 description 1
- 235000010576 Artemisia cina Nutrition 0.000 description 1
- 235000006008 Brassica napus var napus Nutrition 0.000 description 1
- 235000001169 Brassica oleracea var oleracea Nutrition 0.000 description 1
- 241001674939 Caulanthus Species 0.000 description 1
- 235000009024 Ceanothus sanguineus Nutrition 0.000 description 1
- 244000281762 Chenopodium ambrosioides Species 0.000 description 1
- 235000000509 Chenopodium ambrosioides Nutrition 0.000 description 1
- 235000007516 Chrysanthemum Nutrition 0.000 description 1
- 244000189548 Chrysanthemum x morifolium Species 0.000 description 1
- 239000005946 Cypermethrin Substances 0.000 description 1
- 240000003553 Leptospermum scoparium Species 0.000 description 1
- 235000015459 Lycium barbarum Nutrition 0.000 description 1
- 244000061176 Nicotiana tabacum Species 0.000 description 1
- 235000002637 Nicotiana tabacum Nutrition 0.000 description 1
- 241000488583 Panonychus ulmi Species 0.000 description 1
- 241000500437 Plutella xylostella Species 0.000 description 1
- 240000008199 Rhododendron molle Species 0.000 description 1
- 241001454293 Tetranychus urticae Species 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 238000012271 agricultural production Methods 0.000 description 1
- 239000012736 aqueous medium Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001555 benzenes Chemical class 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- KAATUXNTWXVJKI-UHFFFAOYSA-N cypermethrin Chemical compound CC1(C)C(C=C(Cl)Cl)C1C(=O)OC(C#N)C1=CC=CC(OC=2C=CC=CC=2)=C1 KAATUXNTWXVJKI-UHFFFAOYSA-N 0.000 description 1
- 229960005424 cypermethrin Drugs 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 230000000857 drug effect Effects 0.000 description 1
- 239000004495 emulsifiable concentrate Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 241000411851 herbal medicine Species 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 239000000693 micelle Substances 0.000 description 1
- 229930014626 natural product Natural products 0.000 description 1
- 210000000582 semen Anatomy 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 235000015398 thunder god vine Nutrition 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 150000003738 xylenes Chemical class 0.000 description 1
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- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention relates to a microemulsion-type plant pesticide and a preparation method. The pesticide is composed of sessile stemona xylene solution, Melia azedarach xylene solution, nicotine, emulsifier, and water-based pesticide synergist. The microemulsion-type plant pesticide has the advantages that the xylene solvent is basically replaced by the water-based pesticide synergist, and the pesticide is dissolved in the xylene solvent in the preparation to achieve the stability of the extracted active ingredients of sessile stemona and Melia azedarach. The proportion of the xylene solvent in the finished product only accounts for less than 10% of the existing EC pesticide, so that the invention can not only reduce environmental pollution, but also can effectively avoid insecure factors in the storage and transportation process caused by the flammability of the EC pesticide. The microemulsion-type plant pesticide contains ammonium nitrate and ammonium phosphate which can directly form the mixed fertilizer, and plays a positive role in promoting crop production. Based on tests, the cost performance of the pesticide is better than the existing beta-cypermethrin, fenvalerate and other micro-emulsions.
Description
Technical field
The invention belongs to crops pesticide, relate to a kind of microemulsion-type plant pesticide and preparation method thereof.
Background technology
In China's agricultural production,, also make the crops residue of pesticide become the outstanding problem that poses a health risk because natural environment has not only been polluted in the use of a large amount of uses, particularly highly toxic pesticide of chemical pesticide.Therefore adopting the insecticide of low toxicity that natural products constitutes, noresidue, no pesticide resistance, is the effective ways of present substituting chemical pesticide.
The application for a patent for invention of publication number 1111478A " polynary Chinese herbal medicine insecticide and preparation method thereof " discloses following technical scheme: insecticide is made up of kuh-seng, chrysanthemum cinesariaefolium, the tuber of stemona, the root of langdu, China tree, Rhododendron molle, Semen Strychni, the rhizome of Chinese monkshood, thunder godvine, tobacco, trifoliate jewelvine, hemlock, sweet wormwood and Wormseed.Its preparation method is with above-mentioned each component dehydration, pulverize, soak, filter, multiple slag, boiling, refilter, add emulsifier after the concentration.Though above-mentioned insecticide has lot of advantages, prescription is complicated, and the missible oil that is to use the benzene series solvent to make fully, contaminated environment not only, its combustibility increased also that manufactured goods store and transportation in unsafe factor.
Summary of the invention
The present invention is in order to solve the described technical problem that above-mentioned insecticide exists, and disclose a kind of prescription simply, can alleviate natural botanical insecticide of environmental pollution, storing and transporting security, the significant a kind of micro emulsion formulation of drug effect and preparation method thereof.
The natural botanical insecticide of micro emulsion formulation of the present invention is made up of following components in weight percentage:
Tuber of stemona xylene solution 5-10, China tree xylene solution 5-15, nicotine 1-4, emulsifier 8-18, water-base pesticides potentiating agent 53-81.
The stemonine content of described tuber of stemona xylene solution is 1-2%, and the margosine content of China tree xylene solution is 2-6%, and the pure nicotine content of nicotine is 30-45%.
Described emulsifier is the mixture of non-ionic surface active agent OP-10, OP-4, OP-7, and weight ratio is OP-10: OP-4: OP-7=1: 4: 5.
Described water-base pesticides potentiating agent is made up of following components in weight percentage: ammonium nitrate 4-10, ammonium phosphate 3-10, ethylene glycol ethyl ether 6-8, butyl glycol ether 5-8, mix with the two 16～octadecyl ammonium of anion surfactant chlorination dimethyl by non-ionic surface active agent OP-7, amphoteric surfactant field virtue alkali and to form the synergist emulsifier 20-30 that combined group becomes, water 34-59, synergist is OP-7 with the components by weight of emulsifier: field virtue alkali: the two 16～octadecyl ammonium of chlorination dimethyl=4: 2: 1.
Vegetable insecticide its preparation method of the present invention is made up of following steps:
(1) tuber of stemona is pulverized be meal, drop into alcohol reflux lixiviate jar, drop into the ethanol of purity 75% at 1: 5 by solid-to-liquid ratio, extraction temperature 60-70 ℃, stirred lixiviate 2-3 hour down, filter, get that leaching liquor is standby for the first time;
(2) tuber of stemona filter residue secondary lixiviate of step 1 dropped into by solid-to-liquid ratio 1: 3 in the ethanol of purity 75% stirring and leaching 0.5-1 hour, and extraction temperature 60-70 ℃, filter, get that leaching liquor is standby for the second time;
(3) combining step 1,2 twice leaching liquor, decompression recycling ethanol is concentrated into 1/8 volume under 60-65 ℃ temperature, and smart filter gets tuber of stemona cleaner liquid behind the cooling-sedimentation;
(4) tuber of stemona cleaner liquid with step 3 mixes by 1: 1 weight ratio with solvent xylene, is evaporated to 1/4 volume, stemonine content is that the tuber of stemona xylene solution of 1-2% is standby;
(5) set by step it is standby that the method for (1), (2), (3), (4) prepares the xylene solution of China tree, and margosine content is 1-3%;
(6) with mixed emulsifier, the OP-10: OP-4: OP-7=1: 4: 5 of getting of each component of following weight ratio;
(7) OP-7, field virtue alkali, the two 16～octadecyl ammonium of chlorination dimethyl were mixed with the water-base pesticides potentiating agent emulsifier successively by weight 4: 2: 1; With ammonium nitrate 4-10, the water-soluble 24-59 of ammonium phosphate 3-10, add again ethylene glycol ethyl ether 6-8, butyl glycol ether 5-8, water-base pesticides potentiating agent after mixing with emulsifier 20-30 water-base pesticides potentiating agent,
(8) with the water-base pesticides potentiating agent of the emulsifier of the China tree xylene solution of the tuber of stemona xylene solution of step (4), step (5), step (6), step (7) and nicotine by following percentage by weight mix the tuber of stemona, China tree, nicotine vegetable insecticide, tuber of stemona xylene solution 5-10, China tree xylene solution 5-15, nicotine 1-4, emulsifier 8-18, water-base pesticides potentiating agent 53-81.
Beneficial effect of the present invention and advantage are: stemonine, margosine and nicotine that the present invention forms in the component have known broad spectrum disinfestation effect, and outstanding advantage of the present invention is to have substituted xylene solvent substantially with water-base pesticides potentiating agent, only changes for the stability of active ingredient after the tuber of stemona and the China tree lixiviate to be dissolved in xylene solvent in preparation process.Xylene solvent proportion in manufactured goods is below 10% of present cream pesticide, so the present invention not only can alleviate environmental pollution, also can avoid the storage that the combustibility of cream pesticide brings, the unsafe factor in the transportation effectively.Moreover, the water-base pesticides potentiating agent that the present invention forms in the component can make the present invention become microemulsion, analyze its principle and may be the tuber of stemona and xylene solution of China tree and the basis that emulsifier comes down to prepare emulsifiable concentrate pesticide in the preparation process, but mix composite with the non-ionic surface active agent among the present invention and the water-base pesticides potentiating agent of anion surfactant reasonable combination, making its water-fast xylene solution high degree of dispersion form stable dispersion micelle in aqueous medium is micel, multiple layer of surface activating agent is wrapped up on the surface of micel, therefore makes this insecticide have the interior quality of the external feature and the good stability of microemulsion translucent liquid.Its cloud point temperature measured value is 52 ± 1 ℃, and the dilution of being prepared stores the characteristics that still can keep clear in 3-4 month.This insecticide contains ammonium nitrate, the ammonium phosphate composition of direct formation mixed fertilizer, for crop yield self-evident effect is arranged.Certainly, prove also that by a large amount of tests ammonium nitrate, ammonium phosphate composition also have certain role and influence to the formation of microemulsion.In addition, because the broad spectrum disinfestation of this insecticide is effective, so its ratio of performance to price is better than existing beta-cypermethrin microemulsion, sumicidin microemulsion etc.
Below illustrate this insecticide field and use contrast and experiment.
The example 1:2002 4-9 month is the contrast experiment of Da Xinzhai township, Funing County, Hebei province control apple aphid, two spotted spider mite.
Table 1 control apple aphid
Table 2 control European red mite
Comparative result illustrates that the effect of this insecticide obviously is better than cypermethrin.
Example 2: this insecticide and existing beta-cypermethrin microemulsion are used to prevent and treat the contrast experiment of wild cabbage diamond-back moth, and this insecticide (concentration 1.1%) all dilutes 800 times with beta-cypermethrin microemulsion (concentration 4.5%).3 days these insecticides are respectively 71% and 50.32% with the preventive effect of beta-cypermethrin microemulsion behind the medicine, and behind the medicine 7 days, preventive effect was respectively 91.2% and 80.6%.
Example 3: this insecticide and existing matrine alcohol liquid insecticide are used to prevent and treat the contrast experiment of the little greenery worm of tea tree artificial eye, and this insecticide (concentration 1.1%) all dilutes 800 times with matrine alcohol liquid insecticide (concentration 1%).The spray-on process dispenser repeats 4 times, and behind the medicine 7 days, this insecticide preventive effect still reached 91.7%, and matrine alcohol liquid insecticide preventive effect only is 51.8%
Embodiment
Further specify the present invention below in conjunction with embodiment.
Embodiment 1:
With 100 kilograms of pulverizing of the tuber of stemona is 80 order meal, drops into alcohol reflux lixiviate jar, drops into 500 kilograms of the ethanol of purity 75%, extraction temperature 60-70 ℃, stir lixiviate down 3 hours, and filter, get that leaching liquor is standby for the first time; The lixiviate of tuber of stemona filter residue secondary drops into 300 kilograms of the new ethanol of purity 75%, stirring and leaching 1 hour, and extraction temperature 60-70 ℃, filter, get that leaching liquor is standby for the second time; Merge tuber of stemona leaching liquor twice, decompression recycling ethanol is concentrated into 1/8 volume to nothing alcohol flavor under 60-65 ℃ temperature, and concentrate weight is 100 kilograms, naturally cools to room temperature and sedimentation, and the smart filter of 50 orders gets tuber of stemona cleaner liquid; Tuber of stemona cleaner liquid and solvent xylene mix for 100 kilograms, and temperature 60-80 ℃ is evaporated to 1/4 volume, and getting tuber of stemona xylene solution is 25 kilograms of medicinal extract, and measuring stemonine content with high pressure liquid chromatography (HPLC) is 2%.
With 100 kilograms of pulverizing of China tree is 80 order meal, drops into alcohol reflux lixiviate jar, drops into 500 kilograms of the ethanol of purity 75%, extraction temperature 60-70 ℃, stir lixiviate down 3 hours, and filter, get that leaching liquor is standby for the first time; The lixiviate of China tree filter residue secondary drops into 300 kilograms of the new ethanol of purity 75%, stirring and leaching 1 hour, and extraction temperature 60-70 ℃, filter, get that leaching liquor is standby for the second time; Merge the China tree leaching liquor twice, decompression recycling ethanol is concentrated into 1/8 volume to nothing alcohol flavor under 60-65 ℃ temperature, and concentrate weight is 100 kilograms, naturally cools to room temperature and sedimentation, and the smart filter of 50 orders gets the China tree cleaner liquid; China tree cleaner liquid and solvent xylene mix for 100 kilograms, and temperature 60-80 ℃ is evaporated to 1/4 volume, and getting the China tree xylene solution is 25 kilograms of medicinal extract, and measuring margosine content with high pressure liquid chromatography (HPLC) is 3%.
With non-ionic surface active agent OP-10,2 kilograms, OP-4,8 kilograms, OP-7,10 kilograms of mixed 20 kilograms of emulsifier that get;
With non-ionic surface active agent OP-7,20 kilograms, 5 kilograms of 35 kilograms of emulsifier of synergist that mix to form of 10 kilograms in fragrant alkali in amphoteric surfactant field and cationic surfactant 1821 (mixtures of the two 16-octadecyl ammonium of chlorination dimethyl).
Get 10 kilograms in ammonium nitrate, ammonium phosphate is dissolved in 59 kilograms in water for 10 kilograms, water is running water (down with), adds 6 kilograms of ethylene glycol ethyl ethers, 5 kilograms of butyl glycol ethers and synergist again and is mixed with the water-base pesticides potentiating agent 120 kg for 30 kilograms with emulsifier.
Get 10 kilograms of tuber of stemona xylene solutions, 10 kilograms of China tree xylene solutions, 4 kilograms in the nicotine that commercially available pure nicotine content is 30-45%, 18 kilograms of emulsifier, 81 kilograms of water-base pesticides potentiating agents make 123 kilograms in this insecticide.
Embodiment 2:
With 100 kilograms of pulverizing of the tuber of stemona is 80 order meal, drops into alcohol reflux lixiviate jar, drops into 300 kilograms of the ethanol of purity 75%, extraction temperature 60-70 ℃, stir lixiviate down 2 hours, and filter, get that leaching liquor is standby for the first time; The lixiviate of tuber of stemona filter residue secondary drops into 200 kilograms of the new ethanol of purity 75%, stirring and leaching 0.8 hour, and extraction temperature 60-70 ℃, filter, get that leaching liquor is standby for the second time; Merge tuber of stemona leaching liquor twice, decompression recycling ethanol is concentrated into 1/8 volume to nothing alcohol flavor under 60-65 ℃ temperature, and about 66 kilograms of concentrate weight naturally cools to room temperature and sedimentation, and the smart filter of 50 orders gets tuber of stemona cleaner liquid; Tuber of stemona cleaner liquid and solvent xylene mix for 66 kilograms, and temperature 60-80 ℃ is evaporated to 1/4 volume, and getting tuber of stemona xylene solution is 16.5 kilograms of medicinal extract, and measuring stemonine content with high pressure liquid chromatography (HPLC) is 1.5%.
With 100 kilograms of pulverizing of China tree is 80 order meal, drops into alcohol reflux lixiviate jar, drops into 300 kilograms of the ethanol of purity 75%, extraction temperature 60-70 ℃, stir lixiviate down 2 hours, and filter, get that leaching liquor is standby for the first time; The lixiviate of China tree filter residue secondary drops into 200 kilograms of the new ethanol of purity 75%, stirring and leaching 0.8 hour, and extraction temperature 60-70 ℃, filter, get that leaching liquor is standby for the second time; Merge the China tree leaching liquor twice, decompression recycling ethanol is concentrated into 1/8 volume to nothing alcohol flavor under 60-65 ℃ temperature, and concentrate weight is 66 kilograms, naturally cools to room temperature and sedimentation, and the smart filter of 50 orders gets the China tree cleaner liquid; China tree cleaner liquid and solvent xylene mix for 66 kilograms, and temperature 60-80 ℃ is evaporated to 1/4 volume, and getting the China tree xylene solution is 16.5 kilograms of medicinal extract, and measuring margosine content with high pressure liquid chromatography (HPLC) is 2%.
With non-ionic surface active agent OP-10,2 kilograms, OP-4,8 kilograms, OP-7,10 kilograms of mixed 20 kilograms of emulsifier that get;
With non-ionic surface active agent OP-7,20 kilograms, 5 kilograms of 35 kilograms of emulsifier of synergist that mix to form of 10 kilograms in fragrant alkali in amphoteric surfactant field and cationic surfactant 1821 (mixtures of the two 16-octadecyl ammonium of chlorination dimethyl).
Get 8 kilograms in ammonium nitrate, ammonium phosphate is dissolved in 40 kilograms in water for 8 kilograms, add 7 kilograms of ethylene glycol ethyl ethers, 7 kilograms of butyl glycol ethers and synergist again and be mixed with 95 kilograms of water-base pesticides potentiating agents with 25 kilograms of emulsifier.
Get 8 kilograms of tuber of stemona xylene solutions, 8 kilograms of China tree xylene solutions, 3 kilograms in the nicotine that commercially available pure nicotine content is 30-45%, 13 kilograms of emulsifier, 70 kilograms of water-base pesticides potentiating agents make 102 kilograms in this insecticide.
Embodiment 3
With 100 kilograms of pulverizing of the tuber of stemona is 80 order meal, drops into alcohol reflux lixiviate jar, drops into 100 kilograms of the ethanol of purity 75%, extraction temperature 60-70 ℃, stir lixiviate down 1 hour, and filter, get that leaching liquor is standby for the first time; The lixiviate of tuber of stemona filter residue secondary drops into 100 kilograms of the new ethanol of purity 75%, stirring and leaching 0.5 hour, and extraction temperature 60-70 ℃, filter, get that leaching liquor is standby for the second time; Merge tuber of stemona leaching liquor twice, decompression recycling ethanol is concentrated into 1/8 volume to nothing alcohol flavor under 60-65 ℃ temperature, and 33 kilograms of concentrate weight naturally cool to room temperature and sedimentation, and the smart filter of 50 orders gets tuber of stemona cleaner liquid; Tuber of stemona cleaner liquid and solvent xylene mix for 33 kilograms, and temperature 60-80 ℃ is evaporated to 1/4 volume, and getting tuber of stemona xylene solution is 8.25 kilograms of medicinal extract, and measuring stemonine content with high pressure liquid chromatography (HPLC) is 1%.
With 100 kilograms of pulverizing of China tree is 80 order meal, drops into alcohol reflux lixiviate jar, drops into 100 kilograms of the ethanol of purity 75%, extraction temperature 60-70 ℃, stir lixiviate down 1 hour, and filter, get that leaching liquor is standby for the first time; The lixiviate of China tree filter residue secondary drops into 100 kilograms of the new ethanol of purity 75%, stirring and leaching 0.5 hour, and extraction temperature 60-70 ℃, filter, get that leaching liquor is standby for the second time; Merge the China tree leaching liquor twice, decompression recycling ethanol is concentrated into 1/8 volume to nothing alcohol flavor under 60-65 ℃ temperature, and concentrate weight is 33 kilograms, naturally cools to room temperature and sedimentation, and the smart filter of 50 orders gets the China tree cleaner liquid; China tree cleaner liquid and solvent xylene mix for 33 kilograms, and temperature 60-80 ℃ is evaporated to 1/4 volume, and getting the China tree xylene solution is 8.25 kilograms of medicinal extract, and measuring margosine content with high pressure liquid chromatography (HPLC) is 1%.
With non-ionic surface active agent OP-10,2 kilograms, OP-4,8 kilograms, OP-7,10 kilograms of mixed 20 kilograms of emulsifier that get;
With non-ionic surface active agent OP-7,20 kilograms, 10 kilograms in amphoteric surfactant field virtue alkali and 5 kilograms of synergist that mix to form of cationic surfactant 1821 (mixtures of the two 16-octadecyl ammonium of chlorination dimethyl) are with 35 kilograms of emulsifier.
Get 4 kilograms in ammonium nitrate, ammonium phosphate is dissolved in 24 kilograms in water for 3 kilograms, add 8 kilograms of ethylene glycol ethyl ethers, 8 kilograms of butyl glycol ethers and synergist again and be mixed with 67 kilograms of water-base pesticides potentiating agents with 20 kilograms of emulsifier.
Get 5 kilograms of tuber of stemona xylene solutions, 5 kilograms of China tree xylene solutions, 1 kilogram in the nicotine that commercially available pure nicotine content is 30-45%, 8 kilograms of emulsifier, 53 kilograms of water-base pesticides potentiating agents make 72 kilograms in this insecticide.
Claims (5)
1, a kind of natural botanical insecticide of micro emulsion formulation is characterized in that being made up of following components in weight percentage:
Tuber of stemona xylene solution 5-10, China tree xylene solution 5-15, nicotine 1-4, emulsifier 8-18, water-base pesticides potentiating agent 53-81.
2, natural botanical insecticide according to claim 1 is characterized in that: the stemonine content of described tuber of stemona xylene solution is 1-2%, and the margosine content of China tree xylene solution is 2-6%, and the pure nicotine content of nicotine is 30-45%.
3, natural botanical insecticide according to claim 1 is characterized in that: described emulsifier is the mixture of non-ionic surface active agent OP-10, OP-4, OP-7, and weight ratio is OP-10: OP-4: OP-7=1: 4: 5.
4, natural botanical insecticide according to claim 1, it is characterized in that: described water-base pesticides potentiating agent is made up of following components in weight percentage: ammonium nitrate 4-10, ammonium phosphate 3-10, ethylene glycol ethyl ether 6-8, butyl glycol ether 5-8, by non-ionic surface active agent OP-7, amphoteric surfactant field virtue alkali mixes with the two 16～octadecyl ammonium of anion surfactant chlorination dimethyl and forms the synergist emulsifier 20-30 that combined group becomes, water 34-59, synergist is OP-7 with the components by weight of emulsifier: field virtue alkali: the two 16～octadecyl ammonium of chlorination dimethyl=4: 2: 1.
5, natural botanical insecticide according to claim 1, its preparation method is made up of following steps:
(1) tuber of stemona is pulverized be meal, drop into alcohol reflux lixiviate jar, drop into the ethanol of purity 75% at 1: 5 by solid-to-liquid ratio, extraction temperature 60-70 ℃, stirred lixiviate 2-3 hour down, filter, get that leaching liquor is standby for the first time;
(2) tuber of stemona filter residue secondary lixiviate of step 1 dropped into by solid-to-liquid ratio 1: 3 in the ethanol of purity 75% stirring and leaching 0.5-1 hour, and extraction temperature 60-70 ℃, filter, get that leaching liquor is standby for the second time;
(3) combining step 1,2 twice leaching liquor, decompression recycling ethanol is concentrated into 1/8 volume under 60-65 ℃ temperature, and smart filter gets tuber of stemona cleaner liquid behind the cooling-sedimentation;
(4) tuber of stemona cleaner liquid with step 3 mixes by 1: 1 weight ratio with solvent xylene, is evaporated to 1/4 volume, stemonine content is that the tuber of stemona xylene solution of 1-2% is standby;
(5) set by step it is standby that the method for (1), (2), (3), (4) prepares the xylene solution of China tree, and margosine content is 1-3%;
(6) with mixed emulsifier, the OP-10: OP-4: OP-7=1: 4: 5 of getting of each component of following weight ratio;
(7) OP-7, field virtue alkali, the two 16～octadecyl ammonium of chlorination dimethyl were mixed with the water-base pesticides potentiating agent emulsifier successively by weight 4: 2: 1; With ammonium nitrate 4-10, the water-soluble 24-59 of ammonium phosphate 3-10, add again ethylene glycol ethyl ether 6-8, butyl glycol ether 5-8, water-base pesticides potentiating agent after mixing with emulsifier 20-30 water-base pesticides potentiating agent,
(8) with the water-base pesticides potentiating agent of the emulsifier of the China tree xylene solution of the tuber of stemona xylene solution of step (4), step (5), step (6), step (7) and nicotine by following percentage by weight mix the tuber of stemona, China tree, nicotine vegetable insecticide, tuber of stemona xylene solution 5-10, China tree xylene solution 5-15, nicotine 1-4, emulsifier 8-18, water-base pesticides potentiating agent 53-81.
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| CN 200710059741 CN101390518B (en) | 2007-09-21 | 2007-09-21 | Plant pesticide of micro-emulsion and its preparing method |
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| CN106857571A (en) * | 2016-12-31 | 2017-06-20 | 新昌县云河虫害防治技术开发有限公司 | A kind of composite insecticide |
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| CN1045684A (en) * | 1989-03-20 | 1990-10-03 | 曹先立 | A kind of insecticide that contains margosic toxin |
| CN1123087A (en) * | 1994-11-14 | 1996-05-29 | 李洪新 | Composition of traditional Chinese medicine and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106857571A (en) * | 2016-12-31 | 2017-06-20 | 新昌县云河虫害防治技术开发有限公司 | A kind of composite insecticide |
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