CN1813537A - Piperine insecticide and its preparing method - Google Patents

Piperine insecticide and its preparing method Download PDF

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Publication number
CN1813537A
CN1813537A CN 200510020352 CN200510020352A CN1813537A CN 1813537 A CN1813537 A CN 1813537A CN 200510020352 CN200510020352 CN 200510020352 CN 200510020352 A CN200510020352 A CN 200510020352A CN 1813537 A CN1813537 A CN 1813537A
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China
Prior art keywords
piperine
insecticide
pipering
alcohol
extract
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Pending
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CN 200510020352
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Chinese (zh)
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陈华玲
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Individual
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Individual
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Priority to CN 200510020352 priority Critical patent/CN1813537A/en
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Abstract

The present invention discloses a piperine insecticide and its preparation method. Its composition contains (by weight portion) 0-70 portions of piperine, 0-6 portions of artemisinin, 0-17 portions of lindestrenol, 0.1-3 portions of synergistic agent, 3-11 portions of stabilizing agent, 11-16 portions of surfactant, 0.4-7 portions of preservative, 13-60 portions of organic solvent and 0.08-0.3 portion of pH regulating agent. Said piperine insecticide can obtain obvious effect for killing various injurious insects. Besides, said invention also provides the concrete steps of its preparation method.

Description

Piperine insecticide and preparation method thereof
Technical field
The invention belongs to the botanical biological pesticide field, relate to a kind of piperine insecticide and preparation method thereof particularly.
Background technology
Utilize biological characteristic, i.e. some contained composition of plant, the damage by disease and insect that the control crops are had to has it from ancient times.For the understanding and the application of some composition of plant characteristic,, in the books such as Compendium of Material Medica of China's first pharmacy monograph Shennong's Herbal and Ming Dynasty's Li Shizhen (1518-1593 A.D.), very full and accurate elaboration was arranged all as far back as Eastern Han Dynasty last years of a dynasty or reign.In numerous in ancient times pharmacy monographs, just once mention sweet wormwood, golden cypress, kaladana, rhizome of cyrtomium etc. all has insecticidal properties to our ancestors.
Be to promote the agricultural crops increasing both production and income, in decades, China's agricultural crops chemical pesticide of having to use in a large number.A large amount of uses of chemical pesticide have caused heavy damage to human ecological environment.Develop and applying biological pesticide control diseases and pests of agronomic crop, become a kind of inexorable trend of historical development.
And general botanical pesticide, because of preparation method's simple coarse, make medicine effective ingredient complexity, and be difficult to detect, drug effect is difficult for stable, the insecticide effect is slow, and is not easy according to its drug mechanism and the mutual compatibility of other agricultural chemicals, reaches the research and the application that improve drug effect or enlarge insecticidal spectrum.
Summary of the invention
The present invention is directed to chemical pesticide to having a strong impact on that human ecological environment causes, general plant pesticide drug effect instability, a kind of piperine insecticide that the drug effect effect slowly provides and preparation method thereof.Be characterized in separating from pepper, extract and to have the effective ingredient of insecticidal effect, with pipering, or pipering, qinghaosu and/or fragrant camphor tree alcohol be Main Ingredients and Appearance, and warp preferably insecticides adjuvant carries out organic assembling and is processed into.
Piperine insecticide of the present invention is made (consumption is a weight portion) by following component:
Pipering 0-70 part, qinghaosu 0-6 part, fragrant camphor tree alcohol 0-17 part, synergist 0.1-3 part, stabilizing agent 3-11 part, surfactant 11-16 part, preservative 0.4-7 part, organic solvent 13-60 part, PH conditioning agent 0.08-0.3 part.Wherein qinghaosu, fragrant camphor tree alcohol can be simultaneously zero or single be zero.
Described pipering is with the fruit of pepper and or blade is pulverized, immersion, employing organic solvent extractionprocess or supercritical extraction or ultrasonic extraction method or microwave extraction method, extraction insecticidal activity composition, i.e. pipering from pepper.
Described surfactant contains non-ionic surface active agent and anion surfactant: non-ionic surface active agent is selected at least a in alkylphenol formaldehyde condensation product, bis-phenol polyethers, fatty acid glyceride and derivative, fatty acid glycerine fat, alkyl amine oxide, the basic amine alkoxide for use; Anion surfactant is selected toluenesulfonate, C for use 9-C 12At least a in alcohol APEO, alkylphenol-polyethenoxy sulphate, dialkyl group succinic acid fat sulfinic acid salt, the alkyl naphthalene sulfonate.
Described organic solvent is selected at least a in methyl alcohol, ethanol, formaldehyde, mixed alcohol, acetone, dibutyl ester, dioctyl ester, liquor, gasoline, the diesel oil for use.
Described synergist is selected any in azone, DHS activator, synergy phosphorus, 920, the three fourth phosphorus for use.
Described stabilizing agent is selected any in epoxidized vegetable oil, monomethyl ether, the single ethyl ether for use.
Described PH conditioning agent is selected any in acetic acid, sulfuric acid, phosphoric acid, the sodium carbonate for use.
Described preservative is stupid sodium formate.
Described insecticide is the said any formulation of botanical pesticide.As: wetting powder, cream preparation, suspension formulation etc.
The preparation method of described piperine insecticide
One, preparation pipering
(1). fruit and/or the leaf of pepper are pulverized, with methyl alcohol, ethanol, formaldehyde, mixed alcohol, acetone, dibutyl ester, at least a repeatedly extraction of dioctyl ester;
(2). extract is concentrated at temperature 20-100 ℃, and the time is 3-12 hour, is concentrated into the flowing soaking paste extract;
(3). extract is separated, purifies with thin layer folding method, make pipering.
Two, preparation piperine insecticide
(1). by weight with pipering 0-70 part, qinghaosu 0-6 part, fragrant camphor tree alcohol 0-17 part, organic solvent 13-60 part, adding has in the mixing kettle of agitator, is heated to temperature 20-100 ℃, mixes 3-12 hour;
(2). add surfactant 11-16 part, synergist 0.1-3 part, stabilizing agent 3-11 part, preservative 0.4-7 part, PH conditioning agent 0.08-0.3 part, solvent 13-60 part mixes, and obtains cream preparation.
This piperine insecticide can also adopt other existing botanical pesticide preparation method to make any biopesticide formulation.
With pipering, or pipering, qinghaosu and/or fragrant camphor tree alcohol allocates surfactant into, and antioxidant, stabilizing agent, synergist, anti-photolysis agent, cosolvent, PH conditioning agent, carrier are made the wetting powder of piperine insecticide.
With pipering, or pipering, qinghaosu and/or fragrant camphor tree alcohol allocates surfactant, preservative, stabilizing agent, synergist, organic solvent, PH conditioning agent into, makes the cream preparation of piperine insecticide.
With pipering, or pipering, qinghaosu and/or fragrant camphor tree alcohol allocates surfactant, antioxidant, synergist, anti-photolysis agent, stabilizing agent, organic dark agent into, makes the suspension formulation of piperine insecticide.
The present invention has following advantage:
1. wide spectrum, insecticidal effect efficiently
This piperine insecticide has the various pests in wheat, paddy rice, fruit tree, vegetables, flowers, the forest significantly to be killed and control efficiency.
2. low property poison
Raw material of the present invention derive from natural plant, and particularly pepper is that the mankind are generally edible, safe in utilization.
3. friendly environment, the noresidue characteristic
The pipering penetration is strong, and the biological nature volatilization is very fast, is taken at nature, is used for nature, does not have strong toxic residue spy.
4. not having the three wastes handles
The production process economic security, all lixiviate medicines are coated with whole recovery, and the plant slag after the extraction can be used for crop as fertilizer.
The present invention reaches research and the application that improves drug effect or enlarge insecticidal spectrum according to its drug mechanism and the mutual compatibility of other agricultural chemicals easily.
Embodiment
Embodiment one
Pepper raw material (fruit and/or the leaf of pepper tree) process is cleaned, pulverizes, ground, (pepper raw material and methanol usage weight ratio are 1: 2-8) with the methyl alcohol immersion, repeatedly extract with dibutyl ester again, extract is concentrated for 60 ℃ in temperature, time is 8 hours, be concentrated into flowing soaking paste and extract the spy, this extract separates, purifies, obtains pipering with thin layer folding method.
With pipering 50kg, qinghaosu 2kg, fragrant camphor tree alcohol 3kg, organic solvent 27kg, adding has in the agitator mixing kettle of thermometer, to 80 ℃ of temperature, under agitation mixed 8 hours, add surfactant 13kg, azone 1kg, stabilizing agent 3kg, preservative 1kg, PH conditioning agent 0.2kg, mixing and stirring obtains the piperine insecticide product.
Embodiment two
Pepper raw material (fruit and/or the leaf of pepper tree) is cleaned, pulverizes, uses alcohol immersion, (pepper raw material and ethanol consumption weight ratio are 1: 2-8), and again with acetone, repeatedly extraction; Extract is concentrated for 80 ℃ in temperature, and the time is 5 hours, is concentrated into the flowing soaking paste extract, and this extract separates, purifies, obtains pipering with thin layer chromatography.
With pipering 60kg, organic solvent 40kg, adding has in the agitator mixing kettle of thermometer, to 60 ℃ of temperature, under agitation mixed 6 hours, add surfactant 15kg, synergy phosphorus 1, stabilizing agent 4kg, preservative 1kg, PH conditioning agent 0.1kg, mixing and stirring obtains the piperine insecticide product.
Embodiment three
(pepper raw material and ethanol consumption weight ratio are 1: 2-8) through cleaning, pulverize, soaking with mixed alcohol with pepper raw material (fruit and/or the leaf of pepper tree), repeatedly extract with dioctyl ester again, extract is concentrated for 90 ℃ in temperature, time is 3 hours, be concentrated into the flowing soaking paste extract, this extract separates, purifies, makes pipering with thin layer folding method.
With pipering 40kg, fragrant camphor tree alcohol 10kg, organic solvent 50kg, adding has in the agitator mixing kettle of thermometer, under agitation mixed 4 hours to 90 ℃ of temperature, add surfactant 16kg, DHS activator 0.5kg, stabilizing agent 10kg, preservative 0.7kg, PH conditioning agent 0.3kg, mixing and stirring obtains the piperine insecticide product.
Embodiment four
Pepper raw material (fruit and/or the leaf of pepper tree) process is cleaned, pulverizes, soaked (pepper raw material and formaldehyde consumption weight ratio are 1: 28) with formaldehyde, repeatedly extract with dibutyl ester again, to extract in temperature and concentrate for 30 ℃, time is 11 hours, be concentrated into the flowing soaking paste extract, extract is separated, purifies with thin layer chromatography, make pipering.
With pipering 20kg, qinghaosu 6kg, organic solvent 53kg, add and have in the agitator mixing kettle of thermometer, to 80 ℃ of temperature, under agitation mixed 8 hours, add surfactant 14kg, 92 02kg, stabilizing agent 9kg, preservative 3kg, PH conditioning agent 0.1kg, mixing and stirring obtains the piperine insecticide product.
Embodiment five
Pepper raw material (fruit and/or the leaf of pepper tree) process is cleaned, pulverized, (pepper raw material and formaldehyde amount ratio are 1: 2-8) with the methyl alcohol immersion, repeatedly extract with acetone again, extract is concentrated for 60 ℃ in temperature, time is 8 hours, be concentrated into the flowing soaking paste extract, extract is separated, purifies, makes pipering with thin layer chromatography.
With pipering 58kg, qinghaosu 1kg, fragrant camphor tree alcohol 1kg, organic solvent 33kg, adding has in the agitator mixing kettle of thermometer, to 80 ℃ of temperature, under agitation mixed 8 hours, add surfactant 16kg, three fourth phosphorus 1kg, stabilizing agent 5kg, preservative 0.7kg, PH conditioning agent 0.3kg, mixing and stirring obtains the piperine insecticide product.
Embodiment six
Different with the foregoing description one is, raw material proportioning pipering 35kg, and qinghaosu 5kg, fragrant camphor tree alcohol 5kg, organic solvent 40kg, surfactant 15kg, three fourth phosphorus 2kg, stabilizing agent 7kg, preservative 2.8kg, PH conditioning agent 0.2kg, other is identical.
Embodiment seven
Different with above-mentioned enforcement two is, raw material proportioning pipering 65kg, and organic solvent 20kg, surfactant 16kg, azone 2kg, stabilizing agent 4kg, preservative 5.7kg, PH conditioning agent 0.3kg, other is identical.
Embodiment eight
Different with the foregoing description three is, raw material proportioning pipering 55kg, and fragrant camphor tree alcohol 6kg, organic solvent 35kg,, surfactant 13kg, azone 3kg, stabilizing agent 5kg, preservative 1kg, PH conditioning agent 0.2kg, other is identical.
The foregoing description is to further specifying that the present invention carries out, and can not be interpreted as limiting the scope of the invention, and the person skilled in art can content make some nonessential improvement and adjustment to the present invention according to the present invention.

Claims (10)

1. piperine insecticide, it is characterized in that: it is the component that comprises following weight portion
Pipering 13-70 part, qinghaosu 0-6 part, fragrant camphor tree alcohol 0-17 part, synergist 0.1-3 part, stabilizing agent 3-11 part, surfactant 11-16 part, preservative 0.4-7 part, organic solvent 13-60 part, PH conditioning agent 0.08-0.3 part, wherein qinghaosu, fragrant camphor tree alcohol can be simultaneously zero or single be zero.
2. piperine insecticide according to claim 1, it is characterized in that: described pipering is that fruit of pepper tree and/or leaf are pulverized, soaked, adopt organic solvent extractionprocess, or supercritical extraction, or ultrasonic extraction method, or microwave extraction method, the insecticidal activity composition from extract acquisition pepper, i.e. pipering.
3. piperine insecticide according to claim 1 is characterized in that: described surfactant contains non-ionic surface active agent and anion surfactant; Non-ionic surface active agent is at least a in alkylphenol formaldehyde condensation product, bis-phenol polyethers, fatty acid glyceride and the capable thing that spreads out, fatty acid glycerine fat, alkyl amine oxide, the basic amine alkoxide; Anion surfactant is toluenesulfonate, C 9-C 12At least a in alcohol APEO, alkylphenol-polyethenoxy sulphate, dialkyl group succinic acid fat sulfonate, the alkyl naphthalene sulfonate.
4. piperine insecticide according to claim 1 is characterized in that: described organic solvent is at least a in methyl alcohol, ethanol, formaldehyde, mixed alcohol, acetone, dibutyl ester, dioctyl ester, liquor, gasoline, the diesel oil.
5. piperine insecticide according to claim 1 is characterized in that: described synergist is any in azone, DHS activator, synergy phosphorus, 920, the three fourth phosphorus.
6. piperine insecticide according to claim 1 is characterized in that: described stabilizing agent is any in epoxidized vegetable oil, monomethyl ether, the single ethyl ether.
7. piperine insecticide according to claim 1 is characterized in that: described PH conditioning agent is any in acetic acid, sulfuric acid, phosphoric acid, the sodium carbonate.
8. piperine insecticide according to claim 1 is characterized in that: described insecticide is the said any formulation of botanical pesticide.
9. piperine insecticide according to Claim 8 is characterized in that: described insecticide is wetting powder or cream preparation or suspension formulation, aqua.
10. the preparation method of the described piperine insecticide of claim 9 is characterized in that:
One, preparation pipering
(1). fruit and/or the leaf of pepper are pulverized, with methyl alcohol, ethanol, formaldehyde, at least a immersion of mixed alcohol, again with acetone, dibutyl ester, at least a repeatedly extraction of dioctyl ester;
(2). extract is concentrated at temperature 20-100 ℃, and the time is 3-12 hour, is concentrated into the flowing soaking paste extract;
(3). extract is separated, purifies, makes pipering with thin layer folding method;
Two, preparation piperine insecticide
(1). by weight with pipering 0-70 part, qinghaosu 0-6 part, fragrant camphor tree alcohol 0-17 part, organic solvent 13-60 part, adding has in the mixing kettle of agitator, is heated to temperature 20-100 ℃ and mixes 3-12 hour;
(2). add surfactant 11-16 part, synergist 0.1-3 part, stabilizing agent 3-11 part, preservative 0.4-7 part, PH conditioning agent 0.08-0.3 part mixes, and obtains piperine insecticide.
CN 200510020352 2005-02-06 2005-02-06 Piperine insecticide and its preparing method Pending CN1813537A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN 200510020352 CN1813537A (en) 2005-02-06 2005-02-06 Piperine insecticide and its preparing method

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Application Number Priority Date Filing Date Title
CN 200510020352 CN1813537A (en) 2005-02-06 2005-02-06 Piperine insecticide and its preparing method

Publications (1)

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CN1813537A true CN1813537A (en) 2006-08-09

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105494472A (en) * 2015-12-08 2016-04-20 青岛华仁技术孵化器有限公司 Plant extracted pesticide preventing and controlling Chinese cabbage caterpillar
CN113180050A (en) * 2021-04-26 2021-07-30 江苏省中国科学院植物研究所 Application of piperine as agricultural bactericide

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105494472A (en) * 2015-12-08 2016-04-20 青岛华仁技术孵化器有限公司 Plant extracted pesticide preventing and controlling Chinese cabbage caterpillar
CN113180050A (en) * 2021-04-26 2021-07-30 江苏省中国科学院植物研究所 Application of piperine as agricultural bactericide
CN113180050B (en) * 2021-04-26 2022-04-26 江苏省中国科学院植物研究所 Application of piperine as agricultural bactericide

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Open date: 20060809