CN109430264B - Bactericide composition containing terpene alcohol and chitosan, and preparation method and application thereof - Google Patents
Bactericide composition containing terpene alcohol and chitosan, and preparation method and application thereof Download PDFInfo
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N31/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic oxygen or sulfur compounds
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N31/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic oxygen or sulfur compounds
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
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- A01N43/02—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms
- A01N43/04—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom
- A01N43/14—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom six-membered rings
- A01N43/16—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom six-membered rings with oxygen as the ring hetero atom
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Abstract
The invention discloses a bactericide composition containing terpene alcohol and chitosan, which comprises the following active ingredients in parts by weight: 1-20 parts of terpene alcohol and 1-5 parts of chitosan. Also comprises 1-20 parts of levorotatory alpha-terpineol. According to the invention, the terpene alcohol and the chitosan are compounded, so that the synergistic effect is relatively good, the levorotatory alpha-terpineol, the terpene alcohol and the chitosan are compounded, the effects are complementary, the synergistic effect is obvious, the phytopathogen can be effectively killed, and particularly, the control effect on cucumber downy mildew, pearl plum anthracnose and mango powdery mildew is particularly good.
Description
Technical Field
The invention belongs to the technical field of pesticides, and particularly relates to a bactericide composition containing terpene alcohol and chitosan, and a preparation method and application thereof.
Background
Cucumber downy mildew commonly known as "horse race stem" and "dry leaf", can be damaged by adult plants in the seedling stage, mainly leaves and stems, and is less damaged by tendrils and flower stalks. Cucumber downy mildew is the disease which occurs most commonly and seriously in cucumber cultivation. The disease condition is violent, the disease is serious, the propagation is fast, and if the disease is not prevented and cured in time, destructive loss is caused to the cucumbers.
Longtan pearl plum is a late-maturing good variety bred from local wild plum in Guangxi Tian-Ant county, and 2010 is registered by a geographical sign of an agricultural product of Ministry of agriculture, so that the Longtan pearl plum is evaluated as a 'Guangxi high-quality agricultural product' and has the beauty of 'Li nationality queen', and is one of leading industries in Tian-Ant county. In recent years, anthracnose of pearl plum leaves is seriously attacked, and the disease dangerously damages tender leaves, tender tips and fruits and causes serious loss to the production of the pearl plum. At present, the local medicaments for preventing and treating the anthracnose of the pearl plum are older, such as thiophanate methyl, carbendazim, chlorothalonil and the like, and the medicaments have unsatisfactory drug effect due to the generation of drug resistance, thereby seriously restricting the development of the Longtan pearl plum industry.
Mango is one of famous tropical fruits, is popular with people, and is rich in sugar, protein and crude fiber. The precursors of vitamin a, carotene and vitamin C, are particularly high in mango and are rare in all fruits. Mango powdery mildew mainly damages inflorescence and tender leaves. The main symptoms of the disease are manifested as the appearance of scattered powdery small plaques on the damaged organs, then the plaques gradually expand and combine with each other to form a white powdery mildew layer, and tissues under the mildew layer gradually become brown and necrotize. The harmful fungus belongs to the genus Mycoplasma semiaquilegifolium. At present, the control effect on mango powdery mildew is not particularly ideal, the dosage is large, and the cure rate is low.
Terpene alcohol (Terphineol, CAS number 562-74-3), an extract of Melaleuca alternifolia, is a novel botanical fungicide, and has a biological stimulant function. The biological bactericide has protection and treatment effects, and can prevent and treat plant diseases caused by various fungi and bacteria. Has good control effect on various diseases such as downy mildew, powdery mildew, early blight, late blight, leaf spot and the like of various crops. In addition to controlling fungal diseases, bacterial diseases caused by xanthomonas and pseudomonas can also be controlled. Is safe and harmless to bees and other beneficial insects.
Chitosan (Chltosan), also known as chitin and chitin, is a water-soluble product produced by deacetylation of chitin by concentrated alkaline water, and has a molecular formula: (C)6H11O4N)n. The chitosan can inhibit the growth of pathogenic matter and raise the disease resistance and immunity of crop through altering the structure and function of pathogenic matter cell membrane. In agricultural production, chitosan is an excellent plant growth regulator and broad-spectrum bactericide, and can be used for growth of wheat scab, rice leaf blight, potato ring rot, cotton angular leaf spot, etcHas obvious inhibition effect on propagation and fungal spore germination.
Levo alpha-Terpineol (alpha- (L) -Terpineol) is a compound synthesized by Guangxi Zhuang autonomous region chemical research institute (see Chinese patent No. ZL03178548.4, granted 12.26.2007 and named as a preparation method of levo alpha-Terpineol), has good bactericidal activity and also has good deodorization, moistening and permeability. The biological activity of Guangxi Zhuang autonomous region chemical research institute has been studied in a large quantity, and the result shows that the compound can be applied as a pesticide bactericide or a synergist.
With the implementation of national pesticide and fertilizer reduction policy and the increasingly prominent problems of large pollution, long residue and the like of chemical agents, the development of environment-friendly, efficient and low-toxicity pesticides becomes a current focus. At present, the research and the application of the compounding of 3 active ingredients, namely terpene alcohol, chitosan and levorotatory alpha-terpineol, are not reported in a published document.
Disclosure of Invention
The invention mainly aims to provide a bactericide composition containing terpene alcohol and chitosan, which has good bactericidal effect after the terpene alcohol, the chitosan and the levorotatory alpha-terpineol are compounded, has obvious synergistic effect, and particularly has obvious control effect when being applied to the anthracnose of the pearl plum.
In order to achieve the purpose, the technical scheme of the invention is as follows:
the bactericide composition containing terpene alcohol and chitosan of the invention comprises the following active ingredients in parts by weight: 1-20 parts of terpene alcohol and 1-5 parts of chitosan.
Further, the composition also comprises the following active ingredients in parts by weight: 1-20 parts of levorotatory alpha-terpineol.
Further, the bactericide composition containing terpene alcohol and chitosan comprises the following active ingredients in parts by weight: 5-15 parts of terpene alcohol, 2-4 parts of chitosan and 5-15 parts of levo alpha-terpineol.
Further, the bactericide composition containing terpene alcohol and chitosan is prepared into a liquid preparation by matching with auxiliary materials, and is characterized in that the auxiliary materials comprise: 1-70 parts of solvent, 1-20 parts of surfactant, 0-2 parts of defoaming agent, 1-5 parts of antifreezing agent and 0-3 parts of thickening agent.
Further, the solvent is one or a mixture of more of methanol, ethanol, acetone, ethyl acetate, methyl oleate, cyclohexanone, propanol, solvent oil S100A, fatty acid methyl ester and diethylene glycol butyl ether;
the surfactant is one or a mixture of more of calcium dodecyl benzene sulfonate, phenethyl phenol polyoxyethylene ether, triphenethyl phenol polyoxypropylene polyoxyethylene block polymer, calcium lignosulfonate, alkyl naphthalene sulfonate, fatty alcohol polyoxyethylene ether sulfate, polycarboxylate, polyoxyethylene sorbitan fatty acid ester and alkylphenol polyoxyethylene ether;
the defoaming agent is one or a mixture of more of an organic silicon defoaming agent, a phosphate defoaming agent, butyl phosphate, isobutyl phosphate and higher alcohol;
the antifreezing agent is one or a mixture of more of ethylene glycol, propylene glycol and glycerol;
the thickener is one or more of xanthan gum, arabic gum, gelatin, polyvinyl alcohol, magnesium aluminum silicate and sodium carboxymethylcellulose.
Further, the bactericide composition containing terpene alcohol and chitosan is prepared into a solid preparation by matching with auxiliary materials, and is characterized in that the auxiliary materials comprise: 10-70 parts of inert filler and 1-30 parts of functional auxiliary material;
the functional auxiliary materials comprise one or a mixture of a surfactant, a binder and a disintegrating agent.
Further, the inert filler is one or a mixture of more of attapulgite, diatomite, kaolin, white carbon black, bentonite, light calcium carbonate and talcum powder;
the surfactant is one or a mixture of more of calcium lignosulfonate, sodium p-hydroxyphenyl lignosulfonate, sodium dodecyl benzene sulfonate, sodium dodecyl sulfate, calcium dodecyl benzene sulfonate, alkyl naphthalene sulfonate, sodium lignosulfonate, sodium methylene dinaphthalene sulfonate, sodium lauryl alcohol ether sulfate, sodium fatty alcohol-polyoxyethylene ether sulfonate, polyether sodium sulfonate and phenethyl phenol polyoxyethylene ether;
the adhesive is one or a mixture of starch, polyvinylpyrrolidone, carboxymethyl cellulose, carboxyethyl cellulose, gelatin, xanthan gum and Arabic gum;
the disintegrating agent is one or a mixture of more of urea, sodium sulfate, calcium carbonate, ammonium sulfate, calcium sulfate, sodium chloride, magnesium chloride and sodium bicarbonate.
Further, the preparation method of the solid preparation comprises the following steps:
mixing the raw materials with inert filler, pulverizing into fine powder, adding functional adjuvants, and mixing to obtain powder; or adding appropriate amount of binder to further prepare into granule.
The invention also provides application of the bactericide composition containing terpene alcohol and chitosan in preventing and treating cucumber downy mildew, pearl plum anthracnose and mango powdery mildew.
The invention has the following remarkable effects:
1. the terpene alcohol and the chitosan are compounded, so that the terpene alcohol and the chitosan have better synergistic effect, and the synergistic effect of the terpene alcohol and the chitosan is fully proved by experiments of examples 21-22;
2. the levo alpha-terpineol has better dissolving, wetting and penetrating abilities, so that the adhesion and absorption of terpene alcohol and chitosan on crops can be enhanced, the action rate of the bactericides is improved, the dosage of a pesticide formula can be reduced, and the cost is reduced; the levorotatory alpha-terpineol, the terpene alcohol and the chitosan are compounded, the effects are complementary, the synergistic effect is obvious, the phytopathogen can be effectively killed, and particularly, the bactericidal composition has a good effect on cucumber downy mildew, pearl plum anthracnose and mango powdery mildew;
3. according to the invention, the two compositions which have a certain synergistic effect and are composed of the synergist levorotatory alpha-terpineol, terpene alcohol and chitosan are further mixed, the final composition has a better synergistic effect, as described in example 23, the composition has a very large synergistic effect, the dosage can be further reduced, the composition is compounded for use, the action mechanisms are completely different, and cross resistance cannot be generated;
4. the bactericide composition containing terpene alcohol and chitosan provided by the invention has better stability, improves the sterilization speed and prolongs the lasting period. The terpene alcohol can affect the permeation and barrier effects of the biological cell membrane structure of pathogenic bacteria, and destroy the cell membrane and the cell wall, but the effect is slow; the chitosan is a plant growth regulator and can induce crops to generate resistance factors and improve the disease resistance of the crops; the levorotatory alpha-terpineol is used independently as a bactericide, and has large dosage and short duration; the combination of the three components has good quick-acting performance and long lasting period, and can effectively prevent and treat plant diseases.
Detailed Description
The invention is further illustrated by the following examples. It should be understood that the examples of the present invention are for illustrative purposes and not intended to limit the present invention. Simple modifications of the invention in accordance with its spirit fall within the scope of the claimed invention.
Example 1 (10% terpineol-chitosan-levo α -terpineol microemulsion)
The formula of the raw materials of the embodiment is as follows:
6% of terpene alcohol, 1% of chitosan, 3% of levorotatory alpha-terpineol, 8% of N-methyl pyrrolidone, 6% of sodium dodecyl benzene sulfonate, 12% of alkylaryl polyoxypropylene polyoxyethylene ether, 5% of propylene glycol and the balance of water.
The preparation method of the embodiment comprises the following steps:
terpene alcohol, levo alpha-terpineol, N-methyl pyrrolidone, sodium dodecyl benzene sulfonate, alkyl aryl polyoxypropylene polyoxyethylene ether and propylene glycol are fully stirred and dissolved in a container to prepare a uniform oil phase. Mixing chitosan and water in a container under stirring to obtain a uniform water phase. And then slowly adding the oil phase into the water phase with the formula amount, mixing and stirring for 1 hour to obtain the composition microemulsion with the content of the active ingredients of 10 percent.
Example 2 (22% terpinenol-chitosan-levorotatory alpha-terpineol microemulsion)
The formula of the raw materials of the embodiment is as follows:
10% of terpene alcohol, 2% of chitosan, 10% of levo alpha-terpineol, 14% of chloroform, 5% of calcium dodecyl benzene sulfonate, 3% of phenethyl phenol polyoxyethylene ether, 2% of fatty glyceride, 2% of ethylene glycol, 1% of propylene glycol and the balance of water.
The preparation method of the embodiment comprises the following steps:
terpene alcohol, levo alpha-terpineol, calcium dodecylbenzene sulfonate, phenethyl phenol polyoxyethylene ether, fatty glyceride, ethylene glycol and propylene glycol are fully stirred and dissolved in a container to prepare uniform oil phase. Mixing chitosan and water in a container under stirring to obtain a uniform water phase. And then slowly adding the oil phase into the water phase with the formula amount, mixing and stirring for 1.5 hours to obtain the composition microemulsion with the effective component content of 17 percent.
Example 3 (20% terpenol. chitosan. levo. alpha. -terpineol emulsion in water)
The formula of the raw materials of the embodiment is as follows:
9% of terpene alcohol, 1% of chitosan, 10% of levo alpha-terpineol, 5% of calcium dodecyl benzene sulfonate, 10% of dibenzyl biphenyl polyoxyethylene ether, 10% of xylene, 0.5% of isooctyl alcohol, 1% of ethylene glycol, 1% of sorbitol, 1% of polyvinyl alcohol and the balance of water.
The preparation method of the embodiment comprises the following steps:
sequentially adding xylene, terpene alcohol, levorotatory alpha-terpineol, calcium dodecylbenzene sulfonate, dibenzyl biphenyl polyoxyethylene ether, isooctyl alcohol, ethylene glycol, sorbitol and polyvinyl alcohol into a reaction container, uniformly stirring and completely dissolving to obtain an oil phase, stirring and mixing chitosan and water in the container, and preparing into a uniform water phase. Under the condition of high shearing of a homogenizer (the rotating speed is 4000-.
Example 4 (30% terpineol chitosan levo-terpineol wettable powder)
The formula of the raw materials of the embodiment is as follows:
10% of terpene alcohol, 1% of chitosan, 19% of levorotatory alpha-terpineol, 2% of fatty alcohol-polyoxyethylene ether sodium sulfonate, 2% of calcium lignosulfonate, 4% of calcium dodecylbenzene sulfonate and the balance of white carbon black.
The preparation method of the embodiment comprises the following steps:
firstly, adding white carbon black, terpene alcohol and levorotatory alpha-terpineol into a mixer, uniformly mixing, then sequentially adding chitosan, sodium fatty alcohol-polyoxyethylene ether sulfonate, calcium lignosulfonate and sodium dodecyl benzene sulfate into the mixer, fully mixing, adding the uniformly mixed materials into an air flow pulverizer, and pulverizing until the fineness reaches 325 meshes to obtain the composition wettable powder with the effective component content of 30%.
Example 5 (40% terpenol. chitosan. levo. alpha. -terpineol Water dispersible granules)
The formula of the raw materials of the embodiment is as follows:
20% of terpene alcohol, 2% of chitosan, 18% of levorotatory alpha-terpineol, 4% of sodium lignosulfonate, 2% of alkanolamide polyoxyethylene ether sodium sulfonate, 2% of fatty alcohol polyoxyethylene ether sodium sulfonate, 10% of sulfate starch and the balance of bentonite.
The preparation method of the embodiment comprises the following steps:
the preparation method comprises the steps of firstly adding bentonite, terpene alcohol and levorotatory alpha-terpineol into a mixer, uniformly mixing, then sequentially adding chitosan, sodium lignosulfonate, sodium alkanolamide polyoxyethylene ether sulfonate and sodium fatty alcohol polyoxyethylene ether sulfonate into the mixer, fully mixing, adding the uniformly mixed materials into an airflow pulverizer, pulverizing until the fineness reaches 325 meshes, then adding the pulverized materials into the mixer, and mixing for 1 hour to form the premix with a certain concentration. Mixing sulfate starch and water according to the weight ratio of 1: 2, mixing evenly and fully gelatinizing at 80 ℃. Adding the premix and the gelatinized sulfate starch into an extrusion granulator to prepare water dispersible granules, drying, cooling, screening, inspecting, and packaging finished products.
Example 6 (30% terpene alcohol chitosan levo alpha terpineol dispersible oil suspension)
The formula of the raw materials of the embodiment is as follows:
15% of terpene alcohol, 1% of chitosan, 14% of levorotatory alpha-terpineol, 5% of alkyl naphthalene sulfonate formaldehyde condensate, 4% of castor oil polyoxyethylene ether, 8% of fatty alcohol polyoxyethylene ether, 1% of xanthan gum, 1% of organic bentonite and the balance of methyl oleate.
The preparation method of the embodiment comprises the following steps:
adding alkyl naphthalene sulfonate formaldehyde condensate, castor oil polyoxyethylene ether and fatty alcohol polyoxyethylene ether into methyl oleate, and uniformly mixing; sequentially adding terpene alcohol, chitosan and levorotatory alpha-terpineol into the system under high-speed shearing and stirring, then adding organic bentonite and xanthan gum, and stirring and mixing; and finally, grinding the mixture in a zirconium bead medium of a sand mill until the particle size is only 2-4 mu m, and inspecting to obtain the composition dispersible oil suspending agent with the effective component content of 30%.
Example 7 (30% terpenol-chitosan-levo α -terpineol emulsion in water)
The formula of the raw materials of the embodiment is as follows:
8% of terpene alcohol, 2% of chitosan, 20% of levo alpha-terpineol, 3% of calcium dodecyl benzene sulfonate, 3% of phenethyl phenol polyoxyethylene ether, 5% of solvent oil S-100A and the balance of water.
The preparation method of the embodiment comprises the following steps:
the components are respectively weighed according to the formula ratio, chitosan is firstly added into water to be dissolved to obtain a water phase, then terpene alcohol, levorotatory alpha-terpineol, calcium dodecyl benzene sulfonate and phenethyl phenol polyoxyethylene ether are added into S-100A to be mixed to obtain an oil phase, and finally the oil phase and the water phase are stirred and mixed uniformly to obtain the aqueous emulsion.
Example 8 (29% terpenol. chitosan. levo α -terpineol emulsifiable concentrate)
The formula of the raw materials of the embodiment is as follows:
11% of terpene alcohol, 3% of chitosan, 15% of levo alpha-terpineol, 3% of calcium dodecyl benzene sulfonate, 3% of phenethyl phenol polyoxyethylene ether, 100-A7% of solvent oil and the balance of methanol.
The preparation method of the embodiment comprises the following steps:
the components are respectively weighed according to the formula ratio, the active ingredients are firstly dissolved by a solvent, and then the levorotatory alpha-terpineol and the surfactant are added, stirred and mixed evenly to prepare the missible oil.
Example 9 (31% terpineol chitosan levo-terpineol wettable powder)
The formula of the raw materials of the embodiment is as follows:
15% of terpene alcohol, 5% of chitosan, 11% of levo alpha-terpineol, 9% of sodium methylene dinaphthalene sulfonate, 5% of phenethyl phenol polyoxyethylene ether, 15% of calcium sulfate and the balance of white carbon black.
The preparation method of the embodiment comprises the following steps:
the components are respectively weighed according to the formula ratio, and the active ingredient and the inert ingredient are mixed, ground and crushed, then the functional auxiliary material is added, and the mixture is uniformly mixed to prepare the wettable powder.
Example 10 (26% terpenol-chitosan-levo alpha-terpineol water dispersible granules)
The formula of the raw materials of the embodiment is as follows:
18% of terpene alcohol, 1% of chitosan, 7% of levo alpha-terpineol, 5% of sodium polyether sulfonate, 10% of lignosulfonate, 4% of gelatin, 6% of ammonium sulfate, 5% of light calcium carbonate and the balance of bentonite.
The preparation method of the embodiment comprises the following steps:
the components are respectively weighed according to the formula ratio, and the pesticide active ingredient and the inert ingredient are mixed, ground and crushed, then the functional auxiliary material is added, and the mixture is uniformly mixed to prepare powder. And adding an adhesive into the powder, and granulating by a screw to obtain the water dispersible granule.
Example 11 (11% terpene alcohol chitosan levo alpha terpineol dispersible oil suspension)
The formula of the raw materials of the embodiment is as follows:
7% of terpene alcohol, 3% of chitosan, 1% of levo alpha-terpineol, 7% of isobutyl phosphate, 4% of fatty acid polyoxyethylene ether salt, 5% of alkylphenol polyoxyethylene ether, 3% of gelatin, 4% of ethylene glycol and the balance of methyl oleate.
The preparation method of the embodiment comprises the following steps:
the dispersible oil suspending agent is prepared by respectively weighing the components according to the formula ratio, uniformly mixing and grinding through a sand mill.
Example 12 (12% terpenol-chitosan-levo α -terpineol emulsion in water)
The formula of the raw materials of the embodiment is as follows:
5% of terpene alcohol, 2% of chitosan, 5% of levo alpha-terpineol, 2% of ethanol, 30% of fatty acid methyl ester, 6% of alkylphenol polyoxyethylene ether, 2% of alkyl glycoside and the balance of water.
The preparation method of the embodiment comprises the following steps:
weighing the components according to the formula ratio respectively, mixing terpene alcohol, levorotatory alpha-terpineol, ethanol, fatty acid methyl ester, alkylphenol polyoxyethylene ether and alkyl glycoside to prepare an oil phase, adding chitosan into water to prepare a water phase, adding the oil phase into the water phase under the stirring condition, and putting into a high-shear emulsifying machine for shearing to prepare the aqueous emulsion.
Example 13 (29% terpinenol-chitosan-levorotatory alpha-terpineol microemulsion)
The formula of the raw materials of the embodiment is as follows:
9% of terpene alcohol, 3% of chitosan, 17% of levo alpha-terpineol, 3% of sodium dodecyl benzene sulfonate, 6% of alkylphenol polyoxyethylene ether, 9% of cyclohexanone, 7% of acetone, 4% of isopropanol, 4% of ethylene glycol, 2% of polyvinyl alcohol and the balance of water.
The preparation method of the embodiment comprises the following steps:
weighing the components according to the formula ratio respectively, mixing the pesticide active ingredient, the solvent and the surfactant to prepare an oil phase, adding the other components into water to prepare a water phase, adding the oil phase into the water phase under the stirring condition, putting the mixture into a high-shear emulsifying machine, and filtering the liquid obtained after shearing to prepare the microemulsion.
Example 14 (38% terpenol. chitosan. levo alpha-terpineol Water dispersible granules)
The formula of the raw materials of the embodiment is as follows:
17% of terpene alcohol, 1% of chitosan, 20% of levo alpha-terpineol, 5% of calcium lignosulfonate, 3% of polyoxyethylene sorbitan fatty acid ester, 5% of sodium carboxyethyl cellulose, 1% of Arabic gum, 2% of starch, 3% of magnesium chloride and the balance of white carbon black.
The preparation method of the embodiment comprises the following steps:
the components are respectively weighed according to the formula ratio, and the pesticide active ingredient and the inert ingredient are mixed, ground and crushed, then the functional auxiliary material is added, and the mixture is uniformly mixed to prepare powder. And adding an adhesive into the powder, and granulating by a screw to obtain the water dispersible granule.
Example 15 (12% terpene alcohol chitosan levo alpha terpineol suspension)
The formula of the raw materials of the embodiment is as follows:
8% of terpene alcohol, 2% of chitosan, 2% of levo alpha-terpineol, 2.5% of calcium lignosulfonate, 2% of calcium dodecylbenzene sulfonate, 4% of alkylphenol polyoxyethylene ether, 0.02% of organic silicon, 2% of n-octanol, 4% of ethylene glycol and the balance of water.
The preparation method of the embodiment comprises the following steps:
the components are respectively weighed according to the formula ratio, and the suspending agent is prepared by an ultra-micro grinding method.
Example 16 (10% terpene alcohol chitosan suspension)
The formula of the raw materials of the embodiment is as follows:
7% of terpene alcohol, 3% of chitosan, 7% of polyphosphate, 1% of polycarboxylate, 3% of polyoxyethylene sorbitan fatty acid ester, 0.08% of Arabic gum, 2% of ethylene glycol and the balance of water.
The preparation method of the embodiment comprises the following steps:
adding chitosan, polyphosphate and polycarboxylate into water, and uniformly mixing; sequentially adding terpene alcohol and polyoxyethylene sorbitan fatty acid ester under high-speed shearing and stirring, then adding Arabic gum and ethylene glycol, and stirring and mixing; and finally, grinding the mixture in a zirconium bead medium of a sand mill, and checking to obtain the composition suspending agent with the effective component content of 10%.
Example 17 (7% terpene alcohol chitosan suspension)
The formula of the raw materials of the embodiment is as follows:
5% of terpene alcohol, 2% of chitosan, 5% of alkyl naphthalene sulfonate, 10% of polycarboxylate, 0.1% of xanthan gum, 3% of propylene glycol and the balance of water.
The preparation method of the embodiment comprises the following steps:
and weighing the components according to the formula ratio, fully and uniformly mixing, sanding, analyzing and checking to obtain the suspending agent.
Example 18 (12% terpene alcohol chitosan wettable powder)
The formula of the raw materials of the embodiment is as follows:
9% of terpene alcohol, 3% of chitosan, 6% of sodium p-hydroxyphenyl lignin sulfonate, 5% of phenethyl phenol polyoxyethylene ether, 4% of sodium chloride, 3% of ammonium bicarbonate and the balance of white carbon black.
The preparation method of the embodiment comprises the following steps:
the components are respectively weighed according to the formula ratio, and the pesticide active ingredient and the inert ingredient are mixed, ground and crushed, then the functional auxiliary material is added, and the mixture is uniformly mixed to prepare the wettable powder.
Example 19 (18% terpene alcohol chitosan water dispersible granules)
The formula of the raw materials of the embodiment is as follows:
17% of terpene alcohol, 1% of chitosan, 14% of lauryl sodium sulfate, 2% of lauryl alcohol ether sodium sulfate, 5% of carboxyethyl cellulose, 6% of urea, 5% of magnesium sulfate and the balance of attapulgite.
The preparation method of the embodiment comprises the following steps:
the components are respectively weighed according to the formula ratio, and the pesticide active ingredient and the inert ingredient are mixed, ground and crushed, then the functional auxiliary material is added, and the mixture is uniformly mixed to prepare powder. And adding an adhesive into the powder, and performing screw granulation, cutter cutting and hot air drying to obtain the water dispersible granule.
Example 20 (10% terpene alcohol chitosan emulsion)
The formula of the raw materials of the embodiment is as follows:
8% of terpene alcohol, 2% of chitosan, 5% of calcium dodecyl benzene sulfonate, 9% of phenethyl phenol polyoxyethylene ether, 8% of methanol, 9% of acetone and the balance of solvent naphtha S-100A.
The preparation method of the embodiment comprises the following steps:
the components are respectively weighed according to the formula ratio, the active ingredients are firstly dissolved by a solvent, then a surfactant is added, and the missible oil is prepared after stirring and uniform mixing.
Example 21 (indoor toxicity assay of Pseudoperonospora cubensis Georgi with terpene alcohol, Chitosan and L-alpha-terpineol in different ratios)
Indoor bioassay proves that the synergistic condition of the terpene alcohol, the chitosan and the levorotatory alpha-terpineol after compounding is clear. For indoor bioassay tests, refer to part 3 of NY/T1156.3-2006 indoor bioassay test criteria for pesticides: a dish leaf method for testing for inhibiting cucumber downy mildew pathogen is carried out, cucumber downy mildew pathogen (Pseudoperonospora cubensis) is taken as a test pathogen, fresh cucumber downy mildew leaves are collected from four pond towns in Nanning City of the autonomous region of Guangxi Zhuang, brought back to a laboratory, washed clean dust on the leaves with clear water, and subjected to moisture preservation culture and preservation on in-vitro leaves. The sporangia on the back of the leaf are washed off by deionized water, and a suspension of 1 × 105-1 × 107 sporangia/mL is prepared for inoculation.
Dissolving terpene alcohol and levo alpha-terpineol with proper amount of acetone, dissolving chitosan with proper amount of water, preparing mother liquor with mass concentration of 100mg/L, respectively, and mixing 3 kinds of medicinal liquor according to different mass ratios to obtain mixed liquor with different proportions. Selecting 5-6 true-leaf potted 'Xintai Mici' cucumber plants, and spraying the liquid medicine onto the plants by a sprayer until the liquid medicine runs off. And spraying clear water to the blank control. 3 plants were sprayed per mass concentration. After the leaves are dried, 2 leaves with consistent growth vigor are cut off from each treated 3 plants, and the total number of the leaves is 6; placing the back of the leaf upwards in a culture dish paved with wet filter paper, inoculating 4 drops of 10 mu L sporangium suspension to each leaf, culturing in an illumination incubator at 18-20 ℃ for 7-10 d under 12h illumination/d, and measuring and recording the diameter of the lesion according to the control incidence condition.
According to the survey data, the control effect is calculated according to the following formula:
in the formula:
p-controlling effect
D0Blank control lesion diameter
D1Medicament treatment lesion diameter
And performing linear regression analysis between the preventing effect probability value and the concentration logarithm value to obtain a toxicity regression equation of the terpene alcohol, the chitosan, the levorotatory alpha-terpineol and the mixture thereof for inhibiting cucumber downy mildew germs from infecting cucumber leaves, and accordingly, obtaining the EC50 value and the related coefficient of the terpene alcohol, the chitosan, the levorotatory alpha-terpineol and the mixture thereof for the cucumber downy mildew germs.
The compounding synergy of the bactericide is calculated according to the formula of Wadley (1967) to obtain the synergistic coefficient after mixing different medicaments:
in the formula: a. b and C represent the ratio of terpene alcohol (A), chitosan (B) and levo alpha-terpineol (C) in the mixture; EC50(A), EC50(B) and EC50(C) respectively represent the actually observed EC50 value of A, B, C, EC50(th) represents the theoretical EC50 value of A, B, C three medicaments mixed according to a: B: C, and EC50(ob) is the actually observed EC50 value of A, B, C three bactericides mixed according to a: B: C. SR is more than 1.5, synergy; SR <0.5, antagonism; an SR between 0.5 and 1.5 indicates additive effect.
TABLE 1 toxicity synergism of terpene alcohols, chitosan and levo-alpha-terpineol in combination for cucumber downy mildew
From table 1, it can be seen that: the synergistic mixture ratio range of the terpene alcohol, the chitosan and the levorotatory alpha-terpineol for inhibiting cucumber downy mildew bacteria from infecting cucumber leaves is (1-20) to (1-5) to (1-20).
Example 22 (20% terpineol-chitosan-levo-alpha-terpineol emulsion in water field control of Longtan pearl plum anthracnose)
(1) Test material
20% terpenol-chitosan-levorotatory alpha-terpineol emulsion in water (EW) (Guangxi chemical research institute, mass ratio of 9:1: 10); 9% terpene alcohol Emulsifiable Concentrate (EC) [ stokes (israel) limited ]; 2% chitosan water (AS) (santong co, entrepreneur bio ltd); 20% L-alpha-terpineol Emulsifiable Concentrate (EC) (Guangxi chemical research institute).
(2) Orchard conditions
The test is carried out in a six-row Zhengsuo village Linlintun pearl plum orchard in Guangxi Tian Anthric county, the variety to be tested is a 2-year-old Longtan pearl plum fruit tree, the plant spacing multiplied by the row spacing is 3m multiplied by 5m, the slope is moderate in soil fertility, the growth vigor of the fruit trees is basically the same, and anthracnose in the orchard occurs naturally.
(3) Design of experiments
The test is carried out by setting 20 percent of terpene alcohol, chitosan, levorotatory alpha-terpineol EW60, 90, 120 and 150g of a.i./hm29% terpene alcohol EC150g a.i./hm22% chitosan water agent AS 120g a.i./hm220% L-alpha-terpineol EC800g a.i./hm2And a clear water blank, 8 treatments, each 4 replicates, one plot per 3 plants, randomized block permutation. The XQ-D-16 knapsack electric sprayer produced by a sail filling sprayer factory in the road and bridge area of Taizhou city is used for uniformly spraying and applying the medicines for 3 times in the early stage of the disease attack of the new leaves, wherein the application times are 5, 4, 5, 12 and 5, 19 days in 2017. No other bactericide is applied during the test period, and the orchard is fertilized with water pipeThe management, pest control and weed control are consistent with local production.
(4) Investigation and statistics of drug effect
The test investigation is carried out for 4 times, and the disease development base before the medicine is investigated in 2017, 5 months and 3 days; the survey time 1, 2 and 3 after the drug administration is 12 days in 5 months in 2017, 19 days in 26 days. 3 plants in each cell are investigated, and 20 leaves and 100 leaves in each plant are investigated according to the northeast and the northwest of the east, and the total number of leaves is 300. And (4) visually grading according to a grading standard, recording the total leaf number and the leaf number of each grade of disease, and calculating the average disease index and the average control effect.
The diseased leaf grading method comprises the following steps: level 0: no disease spots; level 1: the area of the lesion spots accounts for less than 5% of the whole leaf area; and 3, level: the lesion area accounts for 6 to 15 percent of the whole leaf area; and 5, stage: the lesion area accounts for 16 to 25 percent of the whole leaf area; and 7, stage: the lesion area accounts for 26-50% of the whole leaf area; and 9, stage: the lesion area accounts for more than 51% of the whole leaf area.
The disease control effect difference between treatments is statistically analyzed by Duncan's new double-pole difference method. The drug effect is investigated and simultaneously the safety visual investigation is carried out on the test specimen.
The calculation formula of the drug effect is as follows:
(5) results and analysis
As can be seen from Table 2, the results of the investigation 8d (5 months and 12 days) after the application of the 1 st application showed 20% terpene alcohol, chitosan, L-alpha-terpineol EW60, 90, 120, 150g a.i./hm2The average control effect of the treatment on the Longtan pearl plum anthracnose is between 37.82 and 56.75 percent, and the difference between the treatment and the control medicament is not obvious. 7d after the 2 nd drug (5 months and 19 days), 20% of terpene alcohol, chitosan and levo alpha-terpineol EW 120g a.i./hm2The control effect of the pesticide is 80.43 percent, is basically equivalent to the control effect (80.38 percent) of 9 percent terpene alcohol EC, and is superior to 2 percent chitinPrevention of glycan AS. After the 3 rd time (5 months and 26 days), 20% of terpene alcohol, chitosan and levo alpha-terpineol EW is at 90g a.i./hm2The control effect on the anthracnose of the pearl plums under the treatment has no significant difference from the control effect of 9 percent terpene alcohol EC, and the control effect is 120 and 150g a.i./hm2The control effect of the treatment is respectively 81.58 percent and 89.55 percent, which are both obviously higher than that of other treatments.
TABLE 220% control effect of terpene alcohol, chitosan, levo alpha-terpineol EW on Longtan pearl plum anthracnose
Note: in the table, different lower case letters in the same column indicate that the difference reaches a significant level (P < 0.05), and different upper case letters indicate that the difference reaches a very significant level (P < 0.01).
In the whole test process, no pesticide damage phenomenon of the medicament to the treated leaves of the pearl plum tree is found.
(6) Summary and discussion
The pesticide is applied at the early stage of disease occurrence to prevent and treat anthracnose of Longtan pearl plum, and in the test, 20% of terpene alcohol, chitosan and levorotatory alpha-terpineol have good prevention and treatment effects, and the prevention effect is improved along with the increase of the concentration of the pesticide liquid. After the 3 rd application, 90-150 g a.i./hm of 20% terpene alcohol, chitosan and levorotation alpha-terpineol2The control effect reaches 72.95-89.55%.
Example 23 (field control of terpene alcohol, Chitosan, L-alpha-terpineol combinations against mango powdery mildew)
The test method comprises the following steps: the test is carried out on a mango garden of fruit willow village in east river of Bai-Hua Tian of Guangxi, wherein mango powdery mildew occurs all the year round, the pesticide composition preparation of the embodiment 1-20 is used as a test medicament, 9% terpene alcohol missible oil and 2% chitosan water are used as control medicaments, 3 mango trees are arranged in each cell area in random block groups, and the treatment is repeated for 4 times. The XQ-D-16 knapsack electric sprayer is adopted for spraying, spraying is started when powdery mildew happens sporadically, spraying is carried out uniformly, first spraying is carried out at the initial stage of disease occurrence, second spraying is carried out 7 days later, the disease condition base number is investigated before spraying, the control effect is investigated 7 days before and after second spraying, and the test results are shown in Table 3:
TABLE 3 field efficacy test of different pharmacological treatments on mango powdery mildew
| Test agent | The dosage of effective components (g/hm)2) | First control effect/%) | Second control effect/%) |
| Example 1 | 120 | 70.5 | 81.9 |
| Example 2 | 120 | 71.6 | 82.6 |
| Example 3 | 120 | 69.8 | 81.7 |
| Example 4 | 120 | 74.3 | 88.5 |
| Example 5 | 120 | 78.5 | 90.4 |
| Example 6 | 120 | 75.4 | 89.6 |
| Example 7 | 120 | 71.8 | 82.8 |
| Example 8 | 120 | 69.5 | 80.7 |
| Example 9 | 120 | 70.5 | 84.2 |
| Example 10 | 120 | 72.5 | 88.6 |
| Example 11 | 120 | 72.9 | 85.7 |
| Example 12 | 120 | 69.1 | 83.5 |
| Example 13 | 120 | 75.2 | 90.6 |
| Example 14 | 120 | 74.6 | 88.1 |
| Example 15 | 120 | 73.6 | 87.3 |
| Example 16 | 120 | 67.3 | 80.6 |
| Example 17 | 120 | 65.6 | 80.1 |
| Example 18 | 120 | 70.1 | 83.4 |
| Example 19 | 120 | 71.2 | 82.5 |
| Example 20 | 120 | 70.5 | 81.4 |
| 9% terpene alcohol emulsifiable concentrate | 150 | 63.8 | 78.2 |
| 2% chitosan water agent | 120 | 31.5 | 44.8 |
The results of the field efficacy test are shown in table 3, and it can be seen from table 3 that in examples 1-20, the second control effect of the pesticide preparations prepared by compounding terpene alcohol and chitosan and compounding both with levorotatory alpha-terpineol on mango powdery mildew exceeds 80%, which is obviously superior to the control agents, namely 9% terpene alcohol emulsifiable concentrate and 2% chitosan aqua. Under the condition of the same mixture ratio of the terpene alcohol and the chitosan, the treatment control effect of each of the examples 11-15 added with the levo alpha-terpineol is respectively higher than that of the examples 16-20 not added with the levo alpha-terpineol, which shows that the addition of the levo alpha-terpineol can lead the mixed preparation of the terpene alcohol and the chitosan to have the synergistic effect.
No phytotoxicity of the bactericidal composition to mango crops is observed in the application range, which shows that the bactericidal composition is good in safety and worthy of popularization and application.
Claims (8)
1. A bactericide composition containing terpene alcohol and chitosan is characterized by comprising the following active ingredients in parts by weight: 1-20 parts of terpene alcohol, 1-5 parts of chitosan and 1-20 parts of levo alpha-terpineol.
2. The bactericidal composition containing terpene alcohol and chitosan according to claim 1, which is characterized by comprising the following active ingredients in parts by weight: 5-15 parts of terpene alcohol, 2-4 parts of chitosan and 5-15 parts of levo alpha-terpineol.
3. The bactericidal composition containing terpene alcohol and chitosan according to claim 1 or 2, which is formulated with an adjuvant to form a liquid preparation, characterized in that: the auxiliary materials comprise 1-70 parts by weight of solvent, 1-20 parts by weight of surfactant, 0-2 parts by weight of defoaming agent, 1-5 parts by weight of antifreezing agent and 0-3 parts by weight of thickening agent.
4. A terpene alcohol-chitosan containing bactericide composition as claimed in claim 3, wherein:
the solvent is one or a mixture of methanol, ethanol, acetone, ethyl acetate, methyl oleate, cyclohexanone, propanol, solvent oil S100A, fatty acid methyl ester and diethylene glycol butyl ether;
the surfactant is one or a mixture of more of calcium dodecyl benzene sulfonate, phenethyl phenol polyoxyethylene ether, tristyryl phenol polyoxypropylene polyoxyethylene block polymer, calcium lignosulfonate, alkyl naphthalene sulfonate, fatty alcohol polyoxyethylene ether sulfate, polycarboxylate, polyoxyethylene sorbitan fatty acid ester and alkylphenol polyoxyethylene ether;
the defoaming agent is one or a mixture of more of an organic silicon defoaming agent, a phosphate defoaming agent, butyl phosphate, isobutyl phosphate and higher alcohol;
the antifreezing agent is one or a mixture of more of ethylene glycol, propylene glycol and glycerol;
the thickener is one or more of xanthan gum, arabic gum, gelatin, polyvinyl alcohol, magnesium aluminum silicate and sodium carboxymethylcellulose.
5. The bactericidal composition containing terpene alcohol and chitosan according to claim 1 or 2, which is formulated with an adjuvant to form a solid preparation, characterized in that: the auxiliary materials comprise 10-70 parts by weight of inert filler and 1-30 parts by weight of functional auxiliary materials;
the functional auxiliary materials comprise one or a mixture of a surfactant, a binder and a disintegrating agent.
6. A bactericidal composition containing terpene alcohol and chitosan according to claim 5, wherein:
the inert filler is one or a mixture of more of attapulgite, diatomite, kaolin, white carbon black, bentonite, light calcium carbonate and talcum powder;
the surfactant is one or a mixture of more of calcium lignosulfonate, sodium p-hydroxyphenyl lignosulfonate, sodium dodecyl benzene sulfonate, sodium dodecyl sulfate, calcium dodecyl benzene sulfonate, alkyl naphthalene sulfonate, sodium lignosulfonate, sodium methylene dinaphthalene sulfonate, sodium lauryl alcohol ether sulfate, sodium fatty alcohol-polyoxyethylene ether sulfonate, polyether sodium sulfonate and phenethyl phenol polyoxyethylene ether;
the adhesive is one or a mixture of starch, polyvinylpyrrolidone, carboxymethyl cellulose, carboxyethyl cellulose, gelatin, xanthan gum and Arabic gum;
the disintegrating agent is one or a mixture of more of urea, sodium sulfate, calcium carbonate, ammonium sulfate, calcium sulfate, sodium chloride, magnesium chloride and sodium bicarbonate.
7. The bactericidal composition containing terpene alcohol and chitosan as set forth in claim 5, wherein the preparation method of the solid preparation comprises the steps of:
mixing the raw materials with inert filler, pulverizing into fine powder, adding functional adjuvants, and mixing to obtain powder; or adding appropriate amount of binder to further prepare into granule.
8. Use of a terpene alcohol, chitosan-containing fungicide composition according to any one of claims 1 to 7 for the control of cucumber downy mildew, pearl plum anthracnose and mango powdery mildew.
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