CN1209967C - Euphorbia-one pesticide and preparing method thereof - Google Patents

Euphorbia-one pesticide and preparing method thereof Download PDF

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Publication number
CN1209967C
CN1209967C CN 02133971 CN02133971A CN1209967C CN 1209967 C CN1209967 C CN 1209967C CN 02133971 CN02133971 CN 02133971 CN 02133971 A CN02133971 A CN 02133971A CN 1209967 C CN1209967 C CN 1209967C
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China
Prior art keywords
ketone
euphorbia
root
shares
pesticide
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Expired - Fee Related
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CN 02133971
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CN1404731A (en
Inventor
刘世贵
高平
潘为高
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Sichuan University
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Sichuan University
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Abstract

The present invention relates to a euphorbia ketone pesticide and a preparation method thereof, which is characterized in that Stellera chamaejasme L. is concentrated into euphorbia ketone extractives in a liquid extract form after being cleaned, ground, soaked in organic solvents and extracted for multiple times, the extraction temperature is from 30 to 95 DEG C, and the time is from 2 to 10 hours; 10 to 55 shares of euphorbia ketone extractives, 0 to 5 shares of nimbin, 0 to 12 shares of motherwort alkaloid and 15 to 55 shares of organic solvents are added in a mixture pot with a stirrer and a thermometer; under the condition of stirring, 8 to 16 shares of surface active agents, 2 to 30 shares of tea sapogenin, 0.2 to 2 shares of laurocapram, 3 to 11 shares of stabilizing agents, 0.5 to 1.5 shares of preservatives and 0.1 to 0.2 shares of pH regulators are added under the temperature between 40 and 100 DEG C and are mixed for 0.5 to 5 hours, and then the substances are continuously stirred and uniformly mixed to obtain products of euphorbia ketone pesticides. The products have obvious disinsection and prevention effects on various pests of homoptera, acarina, etc. in vegetables, fruit trees, flowers, forest trees and field crops.

Description

Euphorbia-one pesticide and preparation method thereof
One, technical field
The present invention relates to a kind of euphorbia-one pesticide and preparation method thereof, belong to the biological agricultural medicine of plant resource field.
Two, background technology
China utilizes the characteristic of plant, promptly utilizes its some contained composition, and have existed since ancient times for the control diseases and pests of agronomic crop.According to record, just appliable plant insects agent waits pest control as crotons before 1800.Just once mentioning plants such as the tuber of stemona, black false hellebore, the root of langdu, kuh-seng has insecticidal properties in 1892 kinds of medicines that the Compendium of Material Medica that the Ming Dynasty 24 years Wanli year (1596) Li Shizhen (1518-1593 A.D.) is write is narrated.
Consult pertinent literature and analysis more as can be known, at present, though, mainly be that it is carried out simple application utilizing Chinese Stellera Root as the existing report of the research of biopesticide.As, how to use as the batching of certain insecticide with the form of crude extract.Chinese patent 00116146.6 disclosed " preparation method of biological broad spectrum insecticide ", this technology principal character is to be raw material with Eupatorium adenophorum and Chinese Stellera Root, trifoliate jewelvine, with a kind of in ethanol, methyl alcohol or propyl alcohol, the acetone or their mixture is solvent, through extract, filter, concentrate, grinding technics produces biological broad spectrum insecticide.This technology constitutes the raw insecticide medicine with the plant crude extract, though the preparation method is cheap, technology is simple, the agricultural chemicals of this technology preparation is because of contained composition complexity, and effective ingredient is difficult to detect, and drug effect is not easy to stablize.Contain the material that people and animals is had big toxicity in the what is more important crude extract; Inclusion is too complicated, is not easy its main insecticide active substance is carried out the research of the mechanism of action, is not easy cooperatively interacting to reach further raising drug effect or to enlarge the research of its insecticidal spectrum according to its Study on mechanism itself and other agricultural chemicals.
Three, summary of the invention
The objective of the invention is provides a kind of euphorbia-one pesticide and preparation method thereof at the deficiencies in the prior art, be characterized in from the poisonous plant root of langdu, separating, extracting natural component with insecticidal effect, low polarity is to nonpolar root of langdu ketone, with root of langdu ketone, nimbin and siberian motherwort alkaloid is main component, carries out organic assembling through preferred insecticides adjuvant and is processed into.
Purpose of the present invention is realized that by following technical measures wherein said raw material umber is parts by weight except that specified otherwise.
The recipe ingredient of euphorbia-one pesticide is:
Root of langdu ketone 10-55 part
Nimbin 0-5 part
Siberian motherwort alkaloid 0-12 part
Surfactant 8-16 part
Tea Saponin 2-30 part
Azone 0.2-2 part
Stabilizing agent 3-11 part
Preservative 0.5-1.5 part
PH conditioning agent 0.1-0.2 part
Organic solvent 15-55 part
Wherein to contain Chinese Stellera Root element-B be 10~25wt% to root of langdu ketone, nimbin and siberian motherwort alkaloid can be simultaneously zero or single be zero.
Surfactant contains non-ionic surface active agent and anion surfactant: non-ionic surface active agent is C 8-C 18Alkylphenol polyoxyethylene, C 12-C 18Fatty alcohol-polyoxyethylene ether; Anion surfactant is alkyl sulfate, C 9-C 12Alcohol APEO, alkylbenzenesulfonate, alkylphenol-polyethenoxy sulphate, alkylnaphthalene sulfonate, fatty acid amide N methyl taurine salt, dialkyl group succinic acid fat sulfonate, C 10-C 18Alpha-alkene sulfonate at least a.
Organic solvent be methyl alcohol, ethanol, propyl alcohol, acetone, n-hexane, benzinum and or chloroform at least a.
Stabilizing agent is an epoxidized vegetable oil, and preservative is a Sodium Benzoate, and the PH conditioning agent is sodium hydroxide or acetic acid.
The preparation method of euphorbia-one pesticide:
1, the preparation of root of langdu ketone
With Chinese Stellera Root clean, pulverize, with ethanol, methyl alcohol, propyl alcohol, acetone, n-hexane, benzinum and or chloroform at least a immersion, repeatedly extract, be concentrated into the root of langdu ketone extract of flowing soaking paste, extracting temperature is 30-95 ℃, time is 2-10 hour, the product that obtains, with thin layer chromatography root of langdu ketone is separated, purifies, with the content of ultraviolet spectrum method test Chinese Stellera Root element-B.
2, the preparation of euphorbia-one pesticide
With root of langdu ketone 10-55 part, nimbin 0-5 part, siberian motherwort alkaloid 0-12 part, organic solvent 15-55 part, add and have in the mixing kettle of agitator and thermometer, in temperature 40-100 ℃, under agitation mixed 0.5-5 hour, and added surfactant 8-16 part, Tea Saponin 2-30 part, azone 0.2-2 part, stabilizing agent 3-11 part, preservative 0.5-1.5 part and PH conditioning agent 0.1-0.2 part.Continue to stir, mix, obtain euphorbia-one pesticide.
Wherein stabilizing agent is an epoxidized vegetable oil, and preservative is a Sodium Benzoate, and the PH conditioning agent is sodium hydroxide or acetic acid.
Used auxiliary agent comprises that surfactant, stabilizing agent, preservative etc. all are existing known technologies among the present invention, can be used, to be these auxiliary agents do not have a negative impact to the realization and the obtaining of excellent results of the present invention of purpose of the present invention its precondition.
The present invention has following advantage:
1. have efficient, broad spectrum activity
Euphorbia-one pesticide has various pests such as the Homoptera of vegetables, fruit tree, flowers, forest and field crop, Tetranychus cinnabarinus and to kill significantly and preventive effect.
2. has hypotoxicity
The present invention has removed the composition poisonous to people and animals in preparation process, the toxicological test result shows through Sichuan Province labour health occupation disease precaution﹠china institution, belongs to " low toxicity ", and people and animals are not had the danger of poisoning, belongs to safe agricultural chemicals.
3. non-environmental-pollution
(1) noresidue
Euphorbia-one pesticide is that a kind of active component molecular weight is little, penetration is strong, biological degradation is fast, comes from nature, and can there be toxic residue in back to nature;
(2) produce the no three wastes;
4. raw material sources are extensive, and are inexpensive, technology is easy, is easy to large-scale production.
Four, embodiment
Below by embodiment the present invention is specifically described; be necessary to be pointed out that at this present embodiment only is used for the present invention is further specified; can not be interpreted as limiting the scope of the invention, the person skilled in the art in this field can make some nonessential improvement and adjustment to the present invention according to the content of the invention described above.
Inventive embodiment
Embodiment 1:
With the Chinese Stellera Root raw material through cleaning, pulverize, with alcohol immersion, backflow lixiviate, carry out repeatedly extraction with acetone again, be concentrated into liquid extract root of langdu ketone extract, with root of langdu ketone 8kg, nimbin 1.2kg, siberian motherwort alkaloid 2.5kg; Organic solvent 44kg, adding have in the mixing kettle of agitator and thermometer, in 70 ℃ of temperature, under agitation mixed 2.5 hours, add surfactant 15kg, Tea Saponin 17kg, Sodium Benzoate 1kg, epoxidized vegetable oil 10kg, azone 0.8kg, PH conditioning agent 0.2kg, mixing and stirring obtains the euphorbia-one pesticide product.
Embodiment 2:
With the Chinese Stellera Root raw material through cleaning, pulverize, with methyl alcohol soak, the backflow lixiviate, carry out repeatedly extraction with benzinum again, be concentrated into liquid extract root of langdu ketone extract, with root of langdu ketone 37kg, organic solvent 40kg, adding have in the mixing kettle of agitator and thermometer, in 50 ℃ of temperature, under agitation mixed 1 hour, add surfactant 8kg, Tea Saponin 9kg, Sodium Benzoate 1kg, epoxidized vegetable oil 5kg, azone 1.5kg, PH conditioning agent 0.2kg, mixing and stirring obtains the euphorbia-one pesticide product.
Embodiment 3:
Chinese Stellera Root raw material process is cleaned, pulverizes, is used mixing material immersion, the backflow lixiviate of methyl alcohol and ethanol, carry out repeatedly extraction with n-hexane again, be concentrated into liquid extract root of langdu ketone extract, with root of langdu ketone 15kg, nimbin 0.5kg, siberian motherwort alkaloid 1.8kg; Organic solvent 45kg, adding have in the mixing kettle of agitator and thermometer, in 80 ℃ of temperature, under agitation mixed 4 hours, add surfactant 23kg, Tea Saponin 9.5kg, Sodium Benzoate 1kg, epoxidized vegetable oil 8kg, azone 1kg, PH conditioning agent 0.2kg, mixing and stirring obtains the euphorbia-one pesticide product.
Embodiment 4:
With the Chinese Stellera Root raw material through cleaning, pulverize, with mixing material immersion, the backflow lixiviate of methyl alcohol with ethanol, carry out repeatedly extraction with benzinum again, be concentrated into liquid extract root of langdu ketone extract, with root of langdu ketone 23kg, nimbin 2.8kg; Organic solvent 30kg, adding have in the mixing kettle of agitator and thermometer, in 70 ℃ of temperature, stir, mixed 1.5 hours, add surfactant 10kg, Tea Saponin 24kg, Sodium Benzoate 1kg, epoxidized vegetable oil 8kg, azone 1kg, PH conditioning agent 0.2kg, mixing and stirring is obtained the euphorbia-one pesticide product.
Embodiment 5:
With the Chinese Stellera Root raw material through cleaning, pulverize, with mixing material immersion, the backflow lixiviate of methyl alcohol with ethanol, carry out repeatedly extraction with benzinum again, be concentrated into liquid extract root of langdu ketone extract, with root of langdu ketone 31kg, siberian motherwort alkaloid 4.8kg; Organic solvent 35kg, adding have in the mixing kettle of agitator and thermometer, stir for 90 ℃ in temperature, mixed 2 hours, add surfactant 8kg, Tea Saponin 13kg, Sodium Benzoate 1kg, epoxidized vegetable oil 6kg, azone 1kg, PH conditioning agent 0.2kg, mixing and stirring is obtained the euphorbia-one pesticide product.

Claims (4)

1. euphorbia-one pesticide is characterized in that this insecticide formulation component is by weight:
Root of langdu ketone 10-55 part
Surfactant 8-16 part
Tea Saponin 2-30 part
Azone 0.2-2 part
Stabilizing agent 3-11 part
Preservative 0.5-1.5 part
PH conditioning agent 0.1-0.2 part
Organic solvent 15-55 part
Wherein to contain Chinese Stellera Root element-B be 10~25wt% to root of langdu ketone.
2. according to the described euphorbia-one pesticide of claim 1, it is characterized in that surfactant contains non-ionic surface active agent and anion surfactant: non-ionic surface active agent is C 8-C 18Alkylphenol polyoxyethylene, C 12-C 18Fatty alcohol-polyoxyethylene ether; Anion surfactant is alkyl sulfate, C 9-C 12Alcohol APEO, alkylbenzenesulfonate, alkylphenol-polyethenoxy sulphate, alkylnaphthalene sulfonate, fatty acid amide N methyl taurine salt, dialkyl group succinic acid fat sulfonate, C 10-C 18The a-alkene sulfonate at least a.
3. according to the described euphorbia-one pesticide of claim 1, it is characterized in that organic solvent is at least a in methyl alcohol, ethanol, propyl alcohol, acetone, n-hexane, benzinum and the chloroform.
4. according to the preparation method of the described euphorbia-one pesticide of claim 1, it is characterized in that:
(1) preparation of root of langdu ketone
With Chinese Stellera Root clean, pulverize, with at least a immersion in etoh solvent, methyl alcohol, propyl alcohol, acetone, n-hexane, benzinum and the chloroform, repeatedly extract, be concentrated into the root of langdu ketone extract of flowing soaking paste, extracting temperature is 30-95 ℃, time is 2-10 hour, the product that obtains, with thin layer chromatography root of langdu ketone is separated, purifies, content with ultraviolet spectrum method test Chinese Stellera Root element-B
(2) preparation of euphorbia-one pesticide
With root of langdu ketone 10-55 weight portion, organic solvent 15-55 weight portion, add and have in the mixing kettle of agitator and thermometer, in temperature 40-100 ℃, under agitation mixed 0.5-5 hour, and added surfactant 8-16 weight portion, Tea Saponin 2-30 weight portion, azone 0.2-2 weight portion, stabilizing agent 3-11 weight portion, preservative 0.5-1.5 weight portion and PH conditioning agent 0.1-0.2 weight portion.Continue to stir, mix, obtain euphorbia-one pesticide,
Wherein stabilizing agent is an epoxidized vegetable oil, and preservative is a Sodium Benzoate, and the PH conditioning agent is sodium hydroxide or acetic acid.
CN 02133971 2002-10-28 2002-10-28 Euphorbia-one pesticide and preparing method thereof Expired - Fee Related CN1209967C (en)

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Application Number Priority Date Filing Date Title
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CN1209967C true CN1209967C (en) 2005-07-13

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1331838C (en) * 2005-07-27 2007-08-15 四川大学 Pesticide uses of compound 4-hydroxy sesquiterpene propyl ester

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101926337B (en) * 2009-12-29 2013-01-09 华南农业大学 Pesticide composite of tea saponin and
CN102484992A (en) * 2010-12-02 2012-06-06 华南农业大学 Synergetic pesticide composition of nimbin and tea saponin
CN103183596B (en) * 2012-11-20 2015-05-06 北京农学院 Novel aliphatic ketone compound having acaricidal activity
CN105165900A (en) * 2015-08-12 2015-12-23 贵阳学院 Biological pesticide missible oil preparation for prevention and control of forest pest Monochamus alternatus

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1331838C (en) * 2005-07-27 2007-08-15 四川大学 Pesticide uses of compound 4-hydroxy sesquiterpene propyl ester

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