CN102318603B - Baicalein surfactant and preparation method thereof - Google Patents
Baicalein surfactant and preparation method thereof Download PDFInfo
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- CN102318603B CN102318603B CN 201110221099 CN201110221099A CN102318603B CN 102318603 B CN102318603 B CN 102318603B CN 201110221099 CN201110221099 CN 201110221099 CN 201110221099 A CN201110221099 A CN 201110221099A CN 102318603 B CN102318603 B CN 102318603B
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Abstract
The invention relates to a baicalein surfactant and a preparation method thereof, and relates to a formula and a preparation method of a botanical surfactant. The baicalein surfactant comprises the following components in percentage by mass: 30-40% of astragalus root extract, 56-66% of solvent, 1-3% of preservative and 1-3% of anti-freezing agent. The preparation method comprises the following steps of: adding the solvent to a mixing kettle, heating, then adding the astragalus root extract in proportion, and stirring and dissolving; and then sequentially adding the preservative and the anti-freezing agent in proportion, sufficiently stirring and uniformly mixing. The surfactant provided by the invention is a novel natural environmentally-friendly pesticide synergistic agent; and when added to diluted solution of glyphosate, water-soluble pesticide, powder and wettable powder, the surfactant can improve the adhesion and permeability of pesticide liquid by reducing the surface tension of the pesticide liquid, improve the pesticide retention amount at the target part, prolong lasting period, improve rainwater washing resistance, improve effective utilization rate of pesticide and reduce use amounts of pesticide and water.
Description
Technical field
The present invention relates to formula of a kind of plant resource surfactant and preparation method thereof.
Background technology
At present, China's chemical control area has reached 2.87 hundred million hm
2Inferior, and with average annual growth 0.13 hundred million hm
2Inferior speed increment, there are every year 1000000 tons of pesticidal preparations, 100,000,000 tons of liquids to spray in the farmland, but pesticide efficacy only has 10%-30%, average level far below developed country 50%, the most of agricultural chemicals that sprays is lost in environment, not only waste a large amount of agricultural chemicals, and cause serious environmental pollution and person poultry poisoning.How to improve pesticide efficacy, reduce the injected volume of agricultural chemicals in non-target environment, become China's agricultural chemicals subject problem demanding prompt solution, the research of the reasonable operation technique of agricultural chemicals is one of focus of present Pesticide Science research.
Total present present situation of China of seeing, do not consider " particularity " of biological target in technique in using agriculture chemical, the liquid of same surface characteristic, blade wetability cotton, wheat, corn, rape, spinach, celery etc. preferably both be used for, also be used for blade and be difficult to moistening paddy rice, wild cabbage, cauliflower etc., cause fluid loss serious, run counter to " target adaptability principle ".Generally adopt large capacity spray technique, the effect understanding mistake to water in dusting.
China's water soluble pesticide desinsection list, dimehypo, jinggangmeisu etc. are the large-tonnage pesticide species of control rice pest, owing to wherein not adding suitable surfactant, stick together the performance extreme difference, most of fluid loss during use, not only affect control efficiency, and serious environment pollution.The dispersant that some pulvis, wetting powder add and wetting agent consumption are too low or be not suitable for, and the liquid after dilution sticks together poor performance.
The present common pesticides of China sprays chemical surfactant and mostly is azone, JFC(C7-C9 alkanol APEO), the surfactant such as thiophene ketone.The discovered in recent years organic silicon surfactant directly is added in agricultural chemicals and sprays, can reduce the surface tension of pesticide solution, reduce the contact angle between pesticide droplet and crop leaf surface, improve the wetting and spreading ability on liquid and biological target surface, more can improve agricultural chemicals service efficiency, reduction agricultural chemicals injected volume and water consumption than azone surfactant.
Aspect the botanical pesticide surfactant, China utilizes cocoa butter and corn to develop alkyl glycoside plant resource surfactant, can with any type surfactant compound, synergistic effect is obvious, with 41% gyphosate solution of alkyl glycoside preparation, demonstrate excellent herbicidal effect.SD, SDP are the natural plant auxiliary agents, are that the natural complex that extracts from plant and high-efficient penetrant etc. are composited, and are nonionic surface active agent, and its main component is the triterpene glycosides compound, has good wetability, permeability, adhesivity; Spray on the weeds blade faces after mixing with weed killer herbicide, or spray at plant leaf surface after mixing with insecticide, bactericide and foliage fertilizer, plant stem-leaf surface formation film can be sprayed, reduce liquid in the loss of plant surface, accelerate the absorption of medicament and the conduction in plant corpus, and have ability to resist splash erosion, thereby improve drug effect, reduce pesticide dosage, reduce costs.Tea Saponin is a kind of plant resource surfactant, is a kind of glycoside compounds that extracts from the seed of plant of theaceae oil tea, is a kind of of saponin, itself insect is had action of contace poison, still has synergistic effect as surfactant and other Mixture Use of Insecticides.
The present invention utilizes the active skull cap components in astragalus root---and triterpenoid saponin development of new plant resource surfactant no matter at raw material sources, or aspect processing technology and formula, is showed no bibliographical information both at home and abroad.
Summary of the invention
The present invention's purpose is to provide a kind ofly can improve pesticide efficacy, reduce dosage and water consumption contain plant resource surfactant formula of baicalein and preparation method thereof.
In order to solve the problems of the technologies described above, the invention provides following technical scheme:
A kind of baicalein surfactant comprises the component of following quality proportioning: astragalus root extract medicinal extract 30%-40%, solvent 56%-66%, preservative 1%-3%, antifreeze 1%-3%;
Described solvent is selected from one or more in methyl alcohol, ethanol, propyl alcohol, normal propyl alcohol, isopropyl alcohol, butanols, n-butanol; Described preservative is selected from a kind of in formaldehyde, benzoic acid, sorbic acid, p-hydroxybenzoate; Described antifreeze is selected from a kind of in ethylene glycol, propane diols, urea, ammonium sulfate, glycerine, sodium chloride, calcium chloride.
Preferably, above-mentioned baicalein surfactant comprises the component of following quality proportioning: astragalus root extract medicinal extract 35%, solvent 60%-90% ethanol 61%, preservative formaldehyde 2%, antifreeze ethylene glycol 2%.
The preparation method of above-mentioned baicalein surfactant, method is as follows: first add solvent in modulation kettle, then heating adds astragalus root extract medicinal extract, stirring and dissolving in proportion; Add successively in proportion again preservative and antifreeze, get final product after fully mixing.
Further, the preparation method of described astragalus root extract medicinal extract is: (1) dry astragalus root is pulverized with cracker, pour in pot for solvent extraction after weighing, the solvent impregnated extraction that adds 8-10 times of amounts in pot for solvent extraction, extract is evaporated to solvent in concentration tank and moisture volatilizes, and gets astragalus root crude extract medicinal extract; (2) astragalus root crude extract medicinal extract solvent heating for dissolving is filtered, and keeps supernatant; Supernatant is evaporated to the moisture evaporate to dryness in concentration tank, namely gets astragalus root extract medicinal extract; Described solvent is selected from one or more of methyl alcohol, ethanol, propyl alcohol, normal propyl alcohol, isopropyl alcohol, butanols, n-butanol.
Further, the method for described solvent impregnated extraction is, dipping extracts 3 times, and each solvent load is identical, and extraction time was respectively 72,48 and 24 hours.
Astragalus membranacus [
A. membranceus(Fish) Bunge.] belong to the pulse family Astragalus, China's main product in Shanxi, the ground such as Gansu, Heilungkiang, the Inner Mongol, be a kind of important traditional Chinese medicine.Plant resource surfactant of the present invention is exactly active skull cap components---the surfactant that triterpenoid saponin develops as raw material in the Astragalus membranacus root, and its comprehensive development and utilization for the traditional Chinese medicine Astragalus membranacus provides new approach.
The physical characteristic of surfactant of the present invention is as follows:
Outward appearance: yellowish-brown transparency liquid, pH:5.5-6.0, proportion (25 ℃): 1.007g/cm
3, viscosity (25 ℃): 11.97mm
2/ s(cst), and index of refraction (25 ℃): 1.4065, cloud point :-36 ℃ (condensation point), water-soluble: (1% aqueous solution) is faint yellow, and is transparent, without precipitation, without supernatant; Surface tension (25 ℃): 30.81mN/m, active ingredient (%): 35.
The field control effectiveness test result shows, is 800ml/667m in 10% gyphosate solution dosage
2, water consumption is 45kg/667m
2Condition under, the surfactant of the present invention that adds different amounts in the gyphosate solution liquid is prevented and kill off lamb's-quarters to it and is had obvious synergistic effect, and its consumption is 2 and during 3ml/L, the strain preventive effect more not the added-time improve respectively 12.8% and 16%, more the added-time does not improve respectively 10.5% and 14% to the fresh weight preventive effect.Under the strain preventive effect of guaranteeing lamb's-quarters and fresh weight preventive effect reach condition more than 90%, add surfactant of the present invention (3ml/L) and can reduce by 12.5%-25% dosage and 33.3%-50% water consumption.
75% tpn wetting powder is prevented and treated early blight of tomato with surfactant of the present invention and leaf mold has obvious synergistic effect, under the 3ml/L consumption, 600 times of liquid to the preventive effect of early blight of tomato more not the added-time improve 10.8%, more the added-time improves 12% to the preventive effect of leaf mold.
Surfactant of the present invention has obvious synergistic effect to 20% dimehypo water solution control wild cabbage black peach aphid and cabbage caterpillar, under the 3ml/L consumption, more not added-time raising 8.8%-12% of preventive effect to black peach aphid in 1-10 days after 300 times of liquid medicines is to the more added-time raising 11.3%-14.4% of preventive effect of cabbage caterpillar.
As seen, patent surfactant of the present invention is a kind of new type natural environmental protection type agricultural chemical synergist, add in the dilution of glyphosate, water soluble pesticide, pulvis and wetting powder, can improve by the surface tension that reduces liquid tackness and the permeability of liquid, improve target site medicament hold-up, extend lasting period and resistance of rainwater washing against, improve pesticide efficacy, reduce dosage and water consumption.On applicability, it can mix with Chu Cao Ji ﹑ Sha Chong Ji ﹑ Sha Jun Ji ﹑ Zhi thing Sheng long Tiao Jie Ji ﹑ foliage fertilizer and biopesticide bucket and use.
Embodiment
Below the preferred embodiments of the present invention are described, should be appreciated that preferred embodiment described herein only is used for description and interpretation the present invention, is not intended to limit the present invention.
One, astragalus root extract medicinal extract preparation
1, take astragalus root, pour in pot for solvent extraction after pulverizing with cracker, add extraction 3 times, extraction time was respectively 72,48 and 24 hours, merge No. 3 times extract, extract reduced pressure concentration (0.06MPa, 45 ℃) to ethanol in concentration tank volatilizes, continue reduced pressure concentration after temperature is increased to 65 ℃, namely get astragalus root crude extract medicinal extract after the moisture evaporate to dryness; Recovery ethanol is standby.
2, with above-mentioned gained astragalus root crude extract medicinal extract with same solvent heating for dissolving (temperature 45 C), under normal temperature standing 1 day, filter, keep supernatant; Precipitation is used solvent heating for dissolving (temperature 45 C) 1 time again, and under normal temperature standing 1 day, filter, the reject filter residue keeps supernatant; Merge 2 times supernatant, supernatant reduced pressure concentration (0.06MPa, 65 ℃) in concentration tank namely gets astragalus root extract medicinal extract to the moisture evaporate to dryness.
Concrete formula and preparation method such as table 1.
Table 1 astragalus root extract medicinal extract Preparation Example table
? | The astragalus root quality | Pulverize the order number | Solvent and quality | Thick extracted extract quality | Essence extracted extract quality |
Embodiment 1 | 150kg | 30 | Methyl alcohol 1200kg | 34.23kg | 30kg |
Embodiment 2 | 175kg | 40 | Normal propyl alcohol 1750 kg | 39.94kg | 35kg |
Embodiment 3 | 200kg | 50 | Butanols 1600kg | 45.64kg | 40kg |
Two, baicalein surfactant preparation
First add solvent in modulation kettle, then heating adds astragalus root extract medicinal extract, stirring and dissolving in proportion; Add successively in proportion again preservative and antifreeze, get final product after fully mixing.
Concrete formula and drug effect result such as table 2.
Table 2 baicalein surfactant Preparation Example table
? | Medicinal extract quality kg | Solvent and quality kg | Preservative and quality kg | Antifreeze and quality kg | Finished product quality kg | Extension rate | Surface tension (mN/m) | Reduce (%) than water |
Embodiment 1 | 30 | Methyl alcohol 66 | Formaldehyde 1 | Sodium chloride 3 | 100 | 50 | 46.21 | 35.72 |
Embodiment 2 | 35 | N-butanol 61 | Benzoic acid 3 | Calcium chloride 1 | 100 | 100 | 46.21 | 35.72 |
Embodiment 3 | 40 | Butanols 56 | Sorbic acid 2 | Glycerine 2 | 100 | 200 | 51.35 | 28.57 |
Embodiment 4 | 33 | Ethanol 63 | P-hydroxybenzoate 1.5 | Ammonium sulfate 2.5 | 100 | 300 | 51.35 | 28.57 |
Embodiment 5 | 38 | Propyl alcohol 58 | Formaldehyde 2.5 | Propane diols 1.5 | 100 | 400 | 61.62 | 14.29 |
Embodiment 6 | 38 | Normal propyl alcohol 58 | Benzoic acid 2.5 | Urea 1.5 | 100 | 500 | 61.62 | 14.29 |
Embodiment 7 | 38 | Isopropyl alcohol 58 | Sorbic acid 2.5 | Ethylene glycol 1.5 | 100 | 600 | 61.62 | 14.29 |
/ | / | / | / | / | / | Water | 71.89 | — |
This emulsion processing technology is easy, and raw material sources are extensive, extracts the recyclable recycling of solvent, and is with low cost, can implement industrialization production fully.
It should be noted that at last: the above only is the preferred embodiments of the present invention, be not limited to the present invention, although with reference to previous embodiment, the present invention is had been described in detail, for a person skilled in the art, it still can be modified to the technical scheme that aforementioned each embodiment puts down in writing, and perhaps part technical characterictic wherein is equal to replacement.Within the spirit and principles in the present invention all, any modification of doing, be equal to replacement, improvement etc., within all should being included in protection scope of the present invention.
Claims (4)
1. a baicalein surfactant, is characterized in that, comprises the component of following quality proportioning:
Astragalus root extract medicinal extract 30%-40%, solvent 56%-66%, preservative 1%-3%, antifreeze 1%-3%;
The preparation method of described astragalus root extract medicinal extract is: (1) dry Astragalus membranacus root is pulverized with cracker, pour in pot for solvent extraction after weighing, the solvent impregnated extraction that adds 8-10 times of amounts in pot for solvent extraction, extract is evaporated to solvent in concentration tank and moisture volatilizes, and gets astragalus root crude extract medicinal extract; (2) with solvent with astragalus root crude extract medicinal extract heating for dissolving, filter, keep supernatant; Supernatant is evaporated to the moisture evaporate to dryness in concentration tank, namely gets astragalus root extract medicinal extract;
Described solvent is selected from one or more in methyl alcohol, ethanol, propyl alcohol, normal propyl alcohol, isopropyl alcohol, butanols, n-butanol;
Described preservative is selected from a kind of in formaldehyde, benzoic acid, sorbic acid, p-hydroxybenzoate;
Described antifreeze is selected from a kind of in ethylene glycol, propane diols, urea, ammonium sulfate, glycerine, sodium chloride, calcium chloride.
2. baicalein surfactant according to claim 1, is characterized in that, comprises the component of following quality proportioning: astragalus root extract medicinal extract 35%, solvent 60%-90% ethanol 61%, preservative formaldehyde 2%, antifreeze ethylene glycol 2%.
3. baicalein surfactant according to claim 1 is characterized in that: the method for described solvent impregnated extraction is, dipping extracts 3 times, and each solvent load is identical, and extraction time was respectively 72,48 and 24 hours.
4. the preparation method of baicalein surfactant claimed in claim 1, is characterized in that, method is as follows: first add solvent in modulation kettle, then heating adds astragalus root extract medicinal extract, stirring and dissolving in proportion; Add successively in proportion again preservative and antifreeze, get final product after fully mixing.
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CN1903030A (en) * | 2005-07-26 | 2007-01-31 | 常其钊 | Plant pesticide surfactant, preparation method and application thereof |
CN101589718A (en) * | 2009-06-18 | 2009-12-02 | 浙江省农业科学院 | A kind of high-content tricyclazole suspending agent and preparation method thereof |
CN101766195A (en) * | 2010-01-29 | 2010-07-07 | 北京清源保生物科技有限公司 | Combination for preventing and treating plant virosis and application thereof |
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CN1903030A (en) * | 2005-07-26 | 2007-01-31 | 常其钊 | Plant pesticide surfactant, preparation method and application thereof |
CN101589718A (en) * | 2009-06-18 | 2009-12-02 | 浙江省农业科学院 | A kind of high-content tricyclazole suspending agent and preparation method thereof |
CN101766195A (en) * | 2010-01-29 | 2010-07-07 | 北京清源保生物科技有限公司 | Combination for preventing and treating plant virosis and application thereof |
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