WO2020103500A1 - 一种柑桔用控梢杀菌剂组合物及其制备方法 - Google Patents

一种柑桔用控梢杀菌剂组合物及其制备方法

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Publication number
WO2020103500A1
WO2020103500A1 PCT/CN2019/100729 CN2019100729W WO2020103500A1 WO 2020103500 A1 WO2020103500 A1 WO 2020103500A1 CN 2019100729 W CN2019100729 W CN 2019100729W WO 2020103500 A1 WO2020103500 A1 WO 2020103500A1
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WIPO (PCT)
Prior art keywords
extract
ethanol
parts
weight
ginger
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Application number
PCT/CN2019/100729
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English (en)
French (fr)
Inventor
王超
韦茂春
杨淑兰
易芬远
李略
黄科润
余青云
方冬林
柯敏
Original Assignee
广西化工研究院有限公司
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Publication of WO2020103500A1 publication Critical patent/WO2020103500A1/zh

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Classifications

    • 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
    • A01N65/00—Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof
    • 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
    • A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
    • A01N25/12—Powders or granules
    • A01N25/14—Powders or granules wettable
    • 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
    • A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/34—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom
    • A01N43/40—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom six-membered rings
    • 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
    • A01N65/00—Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof
    • A01N65/40—Liliopsida [monocotyledons]
    • A01N65/48—Zingiberaceae [Ginger family], e.g. ginger or galangal

Definitions

  • the invention relates to the technical field of pesticides, in particular to a tip control fungicide composition for citrus and a preparation method thereof.
  • Citrus canker disease is a worldwide disease that originates in Asia and occurs most commonly in Asian countries. It is also one of the most common diseases in citrus producing areas in China, especially in Guangdong, Guangxi, Hunan and other citrus producing areas.
  • the disease is a bacterial disease. After the citrus is damaged, crater-like lesions are formed on the leaves, branches, and fruits, with a size of 2-8mm. Later, they cause deciduous and fruit drop, which affects the fruit yield and quality. This disease occurs mostly from early April to late November each year, mainly affecting spring, summer and autumn shoots, with summer and autumn shoots being the most severely damaged.
  • the bacteria can infect plants through stomata, skin pores and wounds.
  • Infested tissue rapidly multiplies, stimulating the expansion of host cells until the tissue cells swell and rupture and die.
  • chemical agents are often used for prevention and control in production.
  • the copper preparations such as Bordeaux mixture, copper oxychloride, copper acetate, etc.
  • antibiotics such as streptomycin sulfate and ribonucleic acid
  • the copper preparations are started to be sprayed about 7 days after spring shoots and summer shoots and autumn shoots. Etc.), etc., spray once every 7-10 days for a total of 3 times.
  • Citrus anthracnose is one of the common and severely harmful diseases in China's citrus producing areas.
  • the disease is mainly caused by organs such as leaves, branches, flowers and fruits of citrus, causing deciduous leaves, dead shoots, flowers, fruits and rotten fruits. Etc., leading to a decline in tree vigor, a reduction in production or even a halt.
  • the disease is a fungal disease caused by anthrax, spread by wind and rain or insect vectors, and infects plant tissues through stomata, skin pores, wounds, or directly penetrates the epidermis.
  • spraying is generally carried out after and within one and a half months after flowering, after spraying and within one and a half months after flowering, spraying every 10 days or so, continuous spraying for 2 to 3 times, between July and August Spray again to prevent falling fruit.
  • the medicament can be used as a 40% solution of 40% carbendazim, a 65% solution of dermosin WP 500 times, a 70% thiophanate-methyl wettable powder 800-1000 times, and a 50% carbendazim 800 times solution.
  • Citrus penicillium and green mold are common and serious diseases that occur before and after citrus harvest. They mainly damage the fruit, causing the fruit to mold and rot.
  • the disease is mainly a fungal disease caused by Penicillium or Chlorella, which invades the citrus fruit through the wound through the spores.
  • the fruit is still mainly treated by chemical agents: the biguanide trioctyl benzene sulfonate salt 40% wettable powder 1000-2000 times liquid + Wanlide 1000-2000 times liquid, 70% thiophanate-methyl wettable powder or 50% carbendazim wettable powder 500 times.
  • control techniques adopted in production include several methods such as fertilizer control, artificial control, fruit control, control and chemical control.
  • fertilizer control the use of fertilizer to control shoots, the fruit to control shoots and the shoot to control shoots is not common in production due to high operation requirements and unstable effects.
  • manual tip control is easy to operate and has good effects, it is time-consuming, labor-intensive, and costly, making it unsuitable for large-scale planting.
  • the chemical control tip is accepted by more and more fruit farmers because of its advantages of quick effect, easy operation and low cost.
  • the chemical agents used for chemical shoot control are mainly divided into two categories: one kind of shoot control agent with herbicide as the main component, and the other kind of shoot control agent with plant growth regulator as the main component.
  • the former has quick effects, it has short efficacy and easy to remain, and it is easy to affect the appearance of the fruit during the fruiting period. Therefore, although there are many similar patented products, it is rarely used in production.
  • Plant growth regulators are widely used in production due to their safe and efficient characteristics, including paclobutrazol, chlormequat, meperazine, ethephon and so on. Compared with other types of plant growth regulators, mepazone has the advantages of mild medicinal effects and can be used during flowering.
  • Methylphenidone also known as ketamine, is an efficient, low-toxic, low-residue plant growth regulator. It is easily absorbed by plants and can inhibit the germination and growth of fruit tree branches. Used in late spring and summer, it can reduce the nutrient consumption caused by the massive germination of branches, so as to achieve the effect of increasing the fruit rate and stabilizing and increasing the yield of fruit trees.
  • meperazine to control the tip can also avoid wounds caused by artificial tip removal, thereby reducing the chance of plant infection by diseases.
  • the invention overcomes the deficiencies of the existing products, and provides a safe, efficient, and environmentally friendly, controllable fungicide composition and preparation method for the citrus cultivation and management process with easy access to raw materials and preparation.
  • the tip control fungicide composition for citrus of the present invention is prepared from raw materials including the following parts by weight: garlic 0.2-10 parts, ginger 0.2-10 parts, dianthus 2-20 parts, eucalyptus leaves 2-40 parts, red 40-300 parts of honeysuckle leaves, 0.2-30 parts of purslane, and 0.01-0.7 parts of meperium.
  • the citrus shoot control fungicide composition includes the following parts by weight of raw materials: garlic 2-5 parts, ginger 2-8 parts, dianthus 4-10 parts, eucalyptus leaves 10-30 parts, 50-260 parts of honeysuckle leaves, 2-25 parts of purslane, and 0.02-0.6 parts of meperium.
  • the processing technology of the garlic is: peeling, washing, and crushing the garlic, and enzymatically hydrolyzing it by the decomposition enzyme contained in the garlic at room temperature for 20-40 minutes, and then adding the equivalent of the enzymolysis product 2-
  • the volume percentage of 6-fold weight parts is 60-100% ethanol.
  • Ultrasonic assisted extraction is carried out for more than 60 minutes at a constant temperature of 30-40 ° C, filtered, and the supernatant is centrifuged to concentrate under reduced pressure and dried to obtain garlic extract.
  • each microwave-assisted extraction process is as follows: microwave heating 20-40 Seconds, after naturally cooling to room temperature, continue to heat for 20-40 seconds, then cool to room temperature again, and so cycle for 3-7 minutes.
  • the processing process of the dianthus is: drying and crushing the dianthus, then adding 8-12 times the weight of the dianthus to the ethanol with a volume percentage of 60-100% and soaking for 2-5 days, stirring every 12 hours for 1 Times, after standing, filter to obtain the crude extract; extract with 8 times by weight of ethanol with a volume percentage of 60-100% for 3 hours, filter while hot, and then use 6 times by weight with a volume percentage of 60-100% Ethanol was leached for 2 hours, filtered while hot, and the two extracted filtrates were combined, concentrated under reduced pressure, and dried to obtain dianthus extract.
  • the processing process of the eucalyptus leaves is as follows: washing, drying and crushing the eucalyptus leaves, and then adding 8-12 times the weight of the eucalyptus leaves by weight and the volume percentage of 60-100% ethanol to soak for 2-5 days , Ultrasonic assisted extraction at 20-40 °C for 10-30 minutes, and then continue to soak for 40-50 hours, vacuum extraction to obtain the extract, concentrated under reduced pressure, dried to obtain eucalyptus leaf extract.
  • the processing technique of the red glandular honeysuckle leaf is: washing, drying and crushing the red glandular honeysuckle leaf, and then adding 10-15 times the weight of the red glandular honeysuckle leaf in a volume percentage of 40-90% ethanol The solution was refluxed 1-3 times at 70-85 ° C for 2 hours each time. After the extracts were combined, concentrated under reduced pressure and dried to obtain the red glandular honeysuckle leaf extract.
  • purslane washing, drying and crushing purslane, and then adding 10-30 times the weight of purslane by weight to 40-90% ethanol to soak 2 -After 4 days, ultrasonically assisted extraction at 45-55 ° C for 20-40 minutes, and then continue to soak for 20-30 hours. Vacuum suction filtration to obtain the extract, concentrated under reduced pressure, and dried Portulaca oleracea extract after drying.
  • citrus tip control fungicide composition is mixed with auxiliary materials to make a wettable powder or water dispersible granules;
  • the auxiliary material is one or a mixture of several of wetting agents, dispersing agents, disintegrating agents, defoaming agents, inert fillers, and binders.
  • the wetting agent is sodium dodecyl sulfate, sodium alkylbenzene sulfonate, sodium lignin sulfonate, sodium lauryl ether sulfate, fatty alcohol polyoxyethylene ether sulfonate, dodecyl sulfate One or a mixture of calcium and calcium lignosulfonate;
  • the dispersant is polyoxyethylene ether carboxylate, polyoxyethylene ether sulfonate, sodium methylenebisnaphthalene sulfonate, lignin sulfonate, naphthalene sulfonate formaldehyde condensate sodium salt, alkylphenol poly Oxyethylene ether ether formaldehyde condensate sulfate, one or a mixture of several;
  • the disintegrant is one or a mixture of polyvinylpyrrolidone, anhydrous ammonium sulfate, and anhydrous sodium sulfate;
  • the defoamer is one of emulsified silicone oil, high-carbon alcohol fatty acid ester compound, polyoxyethylene polyoxypropylene pentaerythritol ether, polyoxyethylene polyoxypropylene amine ether, polyoxypropylene glyceryl ether, polyoxypropylene Species or mixtures of several species;
  • the binder is one or a mixture of vegetable gum, animal gum, sodium hydroxymethyl cellulose, and polyethylene glycol;
  • the inert filler is one or a mixture of diatomaceous earth, clay, kaolin, bentonite, attapulgite, and white carbon black.
  • the method for preparing the tip control fungicide composition includes the following steps:
  • A. Weigh garlic, ginger, dianthus, eucalyptus leaves, red honeysuckle leaves, purslane respectively by weight, and process garlic, ginger, dianthus, eucalyptus leaves, red gland honeysuckle leaves, purslane into garlic extract , Ginger extract, dianthus extract, eucalyptus leaf extract, erythrophylla honeysuckle extract, purslane extract;
  • step B Mix the crude powder of each extract in step B with meperazine and auxiliary materials other than the binder to mix well;
  • step C The mixture prepared in step C is further pulverized to obtain a wettable powder
  • a binder is added, and after mixing and stirring, granulation is performed to obtain a water-dispersible granule.
  • controllable fungicide composition uses it in late spring and summer. When used, dissolve the controllable fungicide composition of the present invention in 100-300 times the water and spray it on the branches of the plant Just dry, leaves and fruits.
  • the present invention has the following significant effects:
  • the present invention effectively uses the bactericidal activity of each natural extract by combining various plant-derived extracts according to a certain ratio, and effectively prevents citrus canker, anthracnose, penicillosis, and green mold.
  • the characteristics of low dosage good effect and little residue.
  • the present invention can also play a role in controlling the growth of branch tips, effectively inhibiting the growth of citrus spring (end) tips and summer tips, which is beneficial to the stable and high yield of citrus.
  • one-time application of pesticides can not only complete disease prevention, but also achieve chemical control of the shoots, save two birds with one stone, save time and labor, and save costs.
  • the raw material dosage of the control fungicide composition of the present invention is: 0.2 g of garlic, 0.2 g of ginger, 2 g of dianthus, 2 g of eucalyptus leaves, 40 g of red honeysuckle leaves, 0.2 g of purslane, and 0.01 g of meperium.
  • the preparation method of the tip control fungicide composition of the present invention includes the following steps:
  • the processing technology of garlic is: peel the garlic, wash it, and mash it.
  • the natural enzymolysis of the decomposition enzyme contained in the garlic itself is carried out at room temperature for 20 minutes, and then the volume percentage equal to 2 times the weight of the enzymolysis product is added.
  • 60 % Ethanol, ultrasonically assisted extraction at a constant temperature of 30 ° C for 60 minutes, filtered, centrifuged to take the supernatant, concentrated under reduced pressure, and dried to obtain garlic extract;
  • each microwave-assisted extraction process is as follows: microwave heating for 20 seconds, after naturally cooling to room temperature, heating is continued for 20 seconds, after Cool to room temperature again, and so circulate for 3 minutes;
  • dianthus drying and crushing dianthus, then adding ethanol equivalent to 8 times the weight of dianthus by volume of 60% ethanol for 2 days, stirring every 12 hours, filtering after standing to obtain crude extract ; Leaching with 8 times by weight of 60% ethanol by volume for 3 hours, filtering while hot, then leaching with 6 times by weight of 60% ethanol by volume for 2 hours, filtering while hot, combining the two extracted filtrates , Carry out decompression concentration and drying to obtain dianthus extract;
  • eucalyptus leaves wash, dry and crush the eucalyptus leaves, then add 60% by volume of ethanol equivalent to 8 times the weight of the eucalyptus leaves, soak for 2 days, ultrasonically assisted extraction at 20 °C for 10 minutes, Then continue to soak for 40 hours, vacuum extract the extract, concentrate it under reduced pressure, and get the extract of eucalyptus leaves after drying;
  • the processing technology of the red glandular honeysuckle leaf is: wash, dry and crush the red glandular honeysuckle leaf, then add 40% volumetric ethanol solution equivalent to 10 times the weight of the red glandular honeysuckle leaf, and reflux at 70 °C 1 Each time, 2 hours each time, after combining the extracts, concentrated under reduced pressure and dried to obtain the red glandular honeysuckle leaf extract;
  • the purslane processing technology is: wash, dry and pulverize the whole plant of purslane, and then add 40% ethanol which is equivalent to 10 times the weight of purslane by volume and soak for 2 days, ultrasonically assisted at 45 °C Extract for 20 minutes, and then continue to soak for 20 hours. Vacuum filter to obtain the extract. After concentration under reduced pressure and drying, the purslane extract is obtained;
  • step B Mix the crude powder of each extract in step B with 0.01g of mepazine, 5g of sodium lauryl sulfate, 3g of polyoxyethylene ether carboxylate, 0.5g of emulsified silicone oil, and 1g of white carbon black, and mix well;
  • step D Using a jet mill to further pulverize the mixture prepared in step C to obtain a wettable powder.
  • the tip control fungicidal composition of the present invention is used in the late spring and summer. When used, the tip control fungicidal composition of the present invention is dissolved in 100 times the water and sprayed onto the branches, leaves and Fruit.
  • the raw material dosage of the shoot control fungicide composition of the present invention is: garlic 0.5g, ginger 0.5g, dianthus 3g, eucalyptus leaves 5g, erythrophylla honeysuckle leaves 50g, purslane 1g, meperium 0.02g.
  • the preparation method of the tip control fungicide composition of the present invention includes the following steps:
  • the processing technology of garlic is: peel the garlic, wash it, and mash it.
  • the natural enzymolysis of the decomposition enzyme contained in the garlic itself is carried out at room temperature for 22 minutes, and then the volume percentage equal to 3 times the weight of the enzymolysis product is added to 65 % Ethanol, ultrasonically assisted extraction for 65 minutes at a constant temperature of 32 ° C, filtered, centrifuged to take the supernatant, concentrated under reduced pressure, and dried to obtain garlic extract;
  • each microwave-assisted extraction process is as follows: microwave heating for 25 seconds, after naturally cooling to room temperature, heating is continued for 25 seconds, after Cool to room temperature again, and cycle for 4 minutes;
  • dianthus drying and crushing dianthus, then adding ethanol equivalent to 9 times the weight of dianthus by volume 65% by volume, soaking for 3 days, stirring once every 12 hours, filtering after standing to obtain crude extract ; Leaching with 8 times by weight of 65% ethanol by volume for 3 hours, filtering while hot, then leaching with 6 times by weight of ethanol by 65% volume for 2 hours, filtering while hot, combining the two extracted filtrates , Carry out decompression concentration and drying to obtain dianthus extract;
  • eucalyptus leaves The processing technology of eucalyptus leaves is as follows: wash, dry and crush eucalyptus leaves, then add ethanol equivalent to 9 times the weight of eucalyptus leaves by 65% by volume and soak for 3 days, ultrasonically assisted extraction at 22 °C for 12 minutes, Then continue to soak for 40 hours, vacuum extract the extract, concentrate it under reduced pressure, and get the extract of eucalyptus leaves after drying;
  • the processing technology of the red glandular honeysuckle leaf is: wash, dry and crush the red glandular honeysuckle leaf, then add an ethanol solution with a volume percentage of 45% which is equivalent to 11 times the weight of the red glandular honeysuckle leaf, and reflux at 72 ° C 2 Each time, 2 hours each time, after the extracts are combined, concentrated under reduced pressure and dried to obtain the red gland honeysuckle extract;
  • the purslane process is as follows: purslane is washed, dried and crushed, and then added with 45% by volume of ethanol which is equivalent to 12 times the weight of purslane and soaked for 3 days, followed by ultrasonic assisted extraction at 46 °C 22 minutes, then continue to soak for 22 hours, vacuum extract the extract, concentrate it under reduced pressure, and get the purslane extract after drying;
  • step B Combine the crude powder of each extract in step B with 0.02g of mepazine, 4g of sodium alkylbenzene sulfonate, 3g of polyoxyethylene ether sulfonate, 0.2g of higher alcohol fatty acid ester complex, and 2g of attapulgite Mix well
  • step D Using a jet mill to further pulverize the mixture prepared in step C to obtain a wettable powder.
  • the tip control fungicide composition of the present invention is used in late spring and summer. When used, the tip control fungicide composition of the present invention is dissolved in 120 times the water and sprayed onto the branches, leaves and Fruit.
  • the raw material dosage of the control fungicide composition of the present invention is: 2g of garlic, 2g of ginger, 4g of dianthus, 10g of eucalyptus leaves, 100g of red honeysuckle leaves, 2g of purslane, and 0.1g of meperium.
  • the preparation method of the tip control fungicide composition of the present invention includes the following steps:
  • 1Garlic processing technology peel the garlic, wash and mash it, enzymatically hydrolyze it at room temperature for 25 minutes, then add 70% ethanol by volume equivalent to 4 times the weight of the enzymolysis product, and ultrasonic wave at a constant temperature of 35 °C Auxiliary extraction for 70 minutes, filtering, centrifugation to take the supernatant under reduced pressure, concentration and drying to obtain garlic extract;
  • each microwave-assisted extraction process is as follows: microwave heating for 30 seconds, after naturally cooling to room temperature, heating is continued for 30 seconds, and then cooling To room temperature, so cycle for 5 minutes;
  • 3Dianthus processing technology Dry and crush dianthus, then add 70% ethanol equivalent to 10 times the weight of dianthus to soak for 4 days, stir once every 12 hours, filter the crude extract after standing; then It was leached with 8 times by weight of 70% ethanol by volume for 3 hours, and filtered while hot, and then extracted by 6 times by weight of 70% ethanol by volume for 2 hours, filtered while hot, and the two extracted filtrates were combined.
  • Dianthus caryophylla extract can be obtained by concentration and drying under reduced pressure;
  • red glandular honeysuckle leaf extract Wash, dry and crush the red glandular honeysuckle leaf, then add 50% volumetric ethanol solution equivalent to 12 times the weight of red glandular honeysuckle leaf, and reflux 3 times at 74 °C , 2 hours each time, after the extracts are combined, concentrated under reduced pressure and dried to obtain the red glandular honeysuckle leaf extract;
  • Portulaca oleracea 6Processing technology of Portulaca oleracea: the whole plant of Portulaca oleracea is washed, dried and crushed, and then added with 50% volumetric alcohol equivalent to 14 times the weight of Portulaca oleracea for 4 days, then ultrasonically assisted at 48 °C Extract for 24 minutes, then continue to soak for 24 hours, vacuum extract the extract, concentrate it under reduced pressure, and get the purslane extract after drying;
  • step B Combine the crude powder of each extract in step B with 0.1 g of mepazine, 6 g of sodium lignosulfonate, 2.5 g of sodium methylenebisnaphthalene sulfonate, 0.1 g of polyoxyethylene polyoxypropylene pentaerythritol ether, and 1.5 g of bentonite Mix well
  • step D Using a jet mill to further pulverize the mixture prepared in step C to obtain a wettable powder.
  • the tip control fungicide composition of the present invention is used in the late spring and summer. When used, the tip control fungicide composition of the present invention is dissolved in 140 times the water and sprayed onto the branches, leaves and Fruit.
  • the raw material dosages of the shoot control fungicide composition of the present invention are: garlic 4g, ginger 4g, dianthus 5g, eucalyptus leaves 15g, erythrophylla honeysuckle leaves 80g, purslane 5g, meperium 0.2g.
  • the preparation method of the tip control fungicide composition of the present invention includes the following steps:
  • 1Garlic processing technology peel the garlic, wash and mash it, enzymatically hydrolyze it at room temperature for 20 minutes, then add 75% by volume of ethanol equivalent to 5 times the weight of the enzymolysis product under constant temperature of 35 °C Ultrasound-assisted extraction for 75 minutes, filtering, centrifugation at 2800r / min for 11 minutes, taking supernatant and concentrating under reduced pressure and drying to obtain garlic extract;
  • Dianthus caryophyllus extract The processing technology of Dianthus: Dry and crush Dianthus, then add 55% volume of ethanol equivalent to 11 times the weight of Dianthus, soak for 5 days, stir once every 12 hours, filter after standing to obtain crude extract; then In turn, leaching with 8% by weight of 75% ethanol for 3 hours, filtering while hot, and then leaching with 6% by weight of 75% ethanol for 2 hours, filtering while hot, combining the two extracted filtrates for Dianthus caryophyllus extract can be obtained by concentration and drying under reduced pressure;
  • red glandular honeysuckle leaf extract leaves wash, dry and crush the red glandular honeysuckle leaf, then add 55% volumetric ethanol solution equivalent to 14 times the weight of red glandular honeysuckle leaf, and reflux once at 76 °C , 2 hours each time, after the extracts are combined, concentrated under reduced pressure and dried to obtain the red glandular honeysuckle leaf extract leaves;
  • Portulaca oleracea the whole plant of Portulaca oleracea is washed, dried and crushed, and then added with 55% volumetric alcohol equivalent to 16 times the weight of Portulaca oleracea for 2 days, and then ultrasonically assisted at 50 °C Extract for 26 minutes, and then continue to soak for 25 hours. Vacuum filter to obtain the extract, concentrate under reduced pressure, and dry to obtain the purslane extract.
  • step B Mix the crude powder of each extract in step B with 2g of meperazine, 4g of sodium lauryl ether sulfate, 4g of lignin sulfonate, 0.8g of polyoxyethylene polyoxypropanol amine ether, and 3g of kaolin.
  • step D Using a jet mill to further pulverize the mixture prepared in step C to obtain a wettable powder.
  • the tip control fungicide composition of the present invention is used in late spring and summer. When used, the tip control fungicide composition of the present invention is dissolved in 160 times of water and sprayed onto the branches, leaves and Fruit.
  • the raw material dosages of the shoot control fungicide composition of the present invention are: 5 g of garlic, 8 g of ginger, 10 g of dianthus, 20 g of eucalyptus leaves, 100 g of red honeysuckle leaf, 10 g of purslane, and 0.3 g of meperium.
  • the preparation method of the tip control fungicide composition of the present invention includes the following steps:
  • 1Garlic processing technology peel the garlic, wash and mash it, enzymatically hydrolyze it at room temperature for 30 minutes, then add 80% ethanol by volume equivalent to 6 times the weight of the enzymolysis product, and ultrasonically at a constant temperature of 36 °C Auxiliary extraction for 80 minutes, filtration, centrifugation to take the supernatant under reduced pressure, concentration and drying to obtain garlic extract;
  • each microwave-assisted extraction process is as follows: microwave heating for 30 seconds, after naturally cooling to room temperature, heating is continued for 30 seconds, and then cooled to At room temperature, so cycle for 7 minutes;
  • Dianthus Dry and crush Dianthus, then add 80% ethanol equivalent to 12 times the weight of Dianthus for 2 days, stir once every 12 hours, filter after standing to obtain crude extract; use 8 Leach 80% ethanol by weight for 3 hours, filter while hot, then extract with 6 times 80% ethanol for 2 hours, filter while hot, combine the two extracted filtrates, concentrate under reduced pressure, and dry Get it
  • red glandular honeysuckle leaf wash, dry and crush the red glandular honeysuckle leaf, then add a volume percentage of 60% ethanol solution equivalent to 15 times by weight of the red glandular honeysuckle leaf, and reflux twice at 78 °C , 2 hours each time, after extracts are combined, concentrated under reduced pressure and dried;
  • step B Mix the crude powder of each extract in step B with 0.3g of methylphenidate, 8g of fatty alcohol polyoxyethylene ether sulfonate, 2g of naphthalenesulfonic acid formaldehyde condensate sodium salt, 1g of polyoxypropylene glyceryl ether, and 2g of clay Uniform
  • step D Using a jet mill to further pulverize the mixture prepared in step C to obtain a wettable powder.
  • the tip control fungicidal composition of the present invention is used in the late spring and summer. When used, the tip control fungicidal composition of the present invention is dissolved in 180 times water and sprayed onto the branches, leaves and Fruit.
  • the raw material dosage of the shoot control fungicide composition of the present invention is: 7 g of garlic, 8 g of ginger, 15 g of dianthus, 30 g of eucalyptus leaves, 200 g of red honeysuckle leaves, 20 g of purslane, and 0.4 g of meperium.
  • the preparation method of the tip control fungicide composition of the present invention includes the following steps:
  • 1Garlic processing technology peel the garlic, wash and mash it, enzymatically hydrolyze it at room temperature for 27 minutes, then add 85% ethanol by volume equivalent to 2 times the weight of the enzymolysis product, and ultrasonic wave at a constant temperature of 38 °C Auxiliary extraction for 85 minutes, filtering, centrifugation to take the supernatant under reduced pressure, concentration and drying to obtain garlic extract;
  • each microwave-assisted extraction process is as follows: microwave heating for 35 seconds, after naturally cooling to room temperature, heating is continued for 35 seconds, and then cooled to At room temperature, so cycle for 3 minutes;
  • Dianthus Dry and crush Dianthus, then add 85% ethanol by volume equivalent to 8 times the weight of Dianthus to soak for 3 days, stir once every 12 hours, filter after standing to obtain crude extract; use 8 After leaching with 85% ethanol by volume for 3 hours, filtering while hot, then leaching with 65% ethanol by volume for 2 hours, filtering while hot, and combining the two extracted filtrates to reduce Concentrate and dry to obtain Dianthus extract;
  • red glandular honeysuckle leaf wash, dry and crush the red glandular honeysuckle leaf, then add 70% volumetric ethanol solution equivalent to 10 times the weight of red glandular honeysuckle leaf, and reflux 3 times at 82 °C , 2 hours each time, after combining the extracts, concentrated under reduced pressure and dried to obtain the red glandular honeysuckle extract;
  • purslane is washed, dried and crushed, and then added with a volume percentage equivalent to 25 times the weight of purslane by 70% ethanol and soaked for 2 days, followed by ultrasonic assisted extraction at 53 ° C for 32 minutes. Then continue to soak for 28 hours, vacuum extract to obtain the extract, purify and dry under reduced pressure to get the purslane extract;
  • step B Combine the crude powder of each extract in step B with 0.4 g of mepazine, 7 g of calcium dodecyl sulfate, 2 g of alkylphenol polyoxyethylene ether formaldehyde condensate sulfate, 0.5 g of polyoxypropylene, and 1 g of diatomaceous earth Mix well
  • step D Using a jet mill to further pulverize the mixture prepared in step C to obtain a wettable powder.
  • the tip control fungicide composition of the present invention is used in late spring and summer. When used, the tip control fungicide composition of the present invention is dissolved in 200 times the water and sprayed onto the branches, leaves and Fruit.
  • the raw material dosage of the shoot control fungicide composition of the present invention is: 8 g of garlic, 9 g of ginger, 18 g of dianthus, 35 g of eucalyptus leaves, 260 g of red honeysuckle leaves, 25 g of purslane, and 0.5 g of meperium.
  • the preparation method of the tip control fungicide composition of the present invention includes the following steps:
  • 1Garlic processing technology peel the garlic, wash and mash it, enzymatically hydrolyze it at room temperature for 29 minutes, then add 95% ethanol by volume equivalent to 4 times the weight of the enzymolysis product, and ultrasonic wave at a constant temperature of 39 °C Auxiliary extraction for 90 minutes, filtration, centrifugation to take the supernatant under reduced pressure, concentration and drying to obtain garlic extract;
  • each microwave-assisted extraction process is as follows: microwave heating for 38 seconds, naturally cooling to room temperature, continue heating for 38 seconds, and then cooling to room temperature, so cycle 4 minute;
  • Dianthus Dry and crush Dianthus, then add 95% volume of ethanol equivalent to 10 times the weight of Dianthus to soak for 3 days, stir once every 12 hours, filter the crude extract after standing; use 8% by volume of 90% ethanol was leached for 3 hours, filtered while hot, and then leached with 6 times by weight of 90% ethanol for 2 hours, filtered while hot, and the two extracted filtrates were combined to reduce Concentrate and dry to obtain Dianthus extract;
  • red glandular honeysuckle leaf wash, dry and crush the red glandular honeysuckle leaf, then add an ethanol solution with a volume percentage of 80% equivalent to 12 times the weight of red glandular honeysuckle leaf, and reflux once at 83 °C , 2 hours each time, after the extracts are combined, concentrated under reduced pressure and dried to obtain the extract of erythrocytes;
  • step B Mix the crude powder of each extract in step B with 0.5g of meperazine, 6g of calcium lignosulfonate, 4g of polyoxyethylene ether carboxylate, 1.5g of polyvinylpyrrolidone, 0.3g of emulsified silicone oil, and 1g of white carbon black. Stir evenly;
  • step D After further pulverizing the mixture prepared in step C with a jet mill, add 0.8 g of vegetable gum, mix and stir evenly, and then granulate with a granulator to prepare a water-dispersible granule.
  • the tip control fungicide composition of the present invention is used in late spring and summer. When used, the tip control fungicide composition of the present invention is dissolved in 220 times the water and sprayed onto the branches, leaves and Fruit.
  • the raw material dosages of the shoot control fungicide composition of the present invention are: garlic 10g, ginger 10g, dianthus 20g, eucalyptus leaves 40g, erythrophylla honeysuckle leaves 300g, purslane 30g, and meperium 0.6g.
  • the preparation method of the tip control fungicide composition of the present invention includes the following steps:
  • 1Garlic processing technology peel the garlic, wash and mash it, enzymatically hydrolyze it at room temperature for 40 minutes, then add 95% ethanol by volume equivalent to 6 times the weight of the enzymolysis product, and ultrasonic wave at a constant temperature of 40 °C Auxiliary extraction for 100 minutes, filtration, centrifugation to take the supernatant under reduced pressure, concentration and drying to obtain garlic extract;
  • each microwave-assisted extraction process is as follows: microwave heating for 40 seconds, after naturally cooling to room temperature, heating is continued for 40 seconds, and then cooled to At room temperature, so cycle for 7 minutes;
  • Dianthus caryophylla extract can be obtained by concentration and drying under reduced pressure;
  • red glandular honeysuckle leaf extract Wash, dry and crush the red glandular honeysuckle leaf, then add an ethanol solution equal to 15 times the weight of the red glandular honeysuckle leaf with a volume percentage of 90%, and reflux 3 times at 85 °C , 2 hours each time, after the extracts are combined, concentrated under reduced pressure and dried to obtain the red glandular honeysuckle leaf extract;
  • step B Combine the crude powder of each extract in step B with 0.6g of methylphenidate, 4g of sodium lauryl sulfate, 3g of polyoxyethylene ether sulfonate, 2.5g of anhydrous ammonium sulfate, and 0.6g of higher alcohol fatty acid ester The compound and 1.5g attapulgite are mixed and mixed evenly;
  • step D After further crushing the mixture prepared in step C with a jet mill, add 1 g of animal gum, mix and stir evenly, and then granulate with a granulator to prepare a water-dispersible granule.
  • the tip control fungicide composition of the present invention is used in late spring and summer. When used, the tip control fungicide composition of the present invention is dissolved in 240 times the water and sprayed onto the branches, leaves and Fruit.
  • the raw material dosage of the shoot control fungicide composition of the present invention is: 10g of garlic, 10g of ginger, 20g of dianthus, 40g of eucalyptus leaves, 300g of red honeysuckle leaves, 30g of purslane, and 0.7g of meperium.
  • the preparation method of the tip control fungicide composition of the present invention includes the following steps:
  • 1Garlic processing technology peel the garlic, wash and mash it, enzymatically hydrolyze it at room temperature for 40 minutes, then add 95% ethanol by volume equivalent to 6 times the weight of the enzymolysis product, and ultrasonic wave at a constant temperature of 40 °C Auxiliary extraction for 100 minutes, filtration, centrifugation to take the supernatant under reduced pressure, concentration and drying to obtain garlic extract;
  • each microwave-assisted extraction process is as follows: microwave heating for 40 seconds, after naturally cooling to room temperature, heating is continued for 40 seconds, and then cooled to At room temperature, so cycle for 7 minutes;
  • Dianthus caryophylla extract can be obtained by concentration and drying under reduced pressure;
  • red glandular honeysuckle leaf extract Wash, dry and crush the red glandular honeysuckle leaf, then add an ethanol solution equal to 15 times the weight of the red glandular honeysuckle leaf with a volume percentage of 90%, and reflux 3 times at 85 °C , 2 hours each time, after the extracts are combined, concentrated under reduced pressure and dried to obtain the red glandular honeysuckle leaf extract;
  • step B Combine the crude powder of each extract in step B with 0.7g of methylphenidate, 5g of sodium alkylbenzenesulfonate, 4g of sodium methylenebisnaphthalenesulfonate, 2g of anhydrous sodium sulfate, and 0.2g of polyoxyethylene polyoxypropylene Pentaerythritol ether and 2g bentonite are mixed and mixed evenly;
  • step D After further pulverizing the mixture prepared in step C with a jet mill, add 2 g of sodium carboxymethyl cellulose, mix and stir evenly, and then granulate with a granulator to prepare a water-dispersible granule.
  • the tip control fungicide composition of the present invention is used in late spring and summer. When used, the tip control fungicide composition of the present invention is dissolved in 260 times water and sprayed onto the branches, leaves and Fruit.
  • the raw material dosage of the control fungicide composition of the present invention is: 0.2 g of garlic, 0.2 g of ginger, 2 g of dianthus, 2 g of eucalyptus leaves, 40 g of red honeysuckle leaves, 0.2 g of purslane, and 0.7 g of meperium.
  • the preparation method of the tip control fungicide composition of the present invention includes the following steps:
  • 1Garlic processing technology peel the garlic, wash and mash it, and enzymatically hydrolyze it at room temperature for 20 minutes, then add 100% ethanol by volume equivalent to 6 times the weight of the enzymolysis product, and ultrasonic wave at a constant temperature of 30 °C Auxiliary extraction for 70 minutes, filtering, centrifugation to take the supernatant under reduced pressure, concentration and drying to obtain garlic extract;
  • each microwave-assisted extraction process is as follows: microwave heating for 20 seconds, after naturally cooling to room temperature, heating is continued for 20 seconds, and then cooled to At room temperature, so cycle for 4 minutes;
  • 3Dianthus processing technology Dry and crush dianthus, then add 100% ethanol equivalent to 8 times the weight of dianthus for 2 days, stir once every 12 hours, filter after standing to obtain crude extract; then It was leached with 8 times by weight of 100% ethanol by volume for 3 hours, and filtered while hot, then 6 times by weight with 100% ethanol by volume for 2 hours, filtered while hot, and the two extracted filtrates were combined.
  • Dianthus caryophylla extract can be obtained by concentration and drying under reduced pressure;
  • red glandular honeysuckle leaf extract Wash, dry and crush the red glandular honeysuckle leaf, then add an ethanol solution with a volume percentage of 90% equivalent to 13 times the weight of the red glandular honeysuckle leaf, and reflux twice at 75 °C , 2 hours each time, after the extracts are combined, concentrated under reduced pressure and dried to obtain the red glandular honeysuckle leaf extract;
  • step B Combine the crude powder of each extract in step B with 0.7g of mepazine, 3g of sodium lignosulfonate, 3g of naphthalenesulfonic acid formaldehyde condensate sodium salt, 2g of anhydrous sodium sulfate, 1g of polyoxyethylene polyoxypropanolamine Ether and 3g kaolin are mixed and mixed evenly;
  • step D After further crushing the mixture prepared in step C with a jet mill, add 2.5 g of polyethylene glycol, mix and stir evenly, and then granulate with a granulator to prepare a water-dispersible granule.
  • the tip control fungicide composition of the present invention is used in the late spring and summer. When used, the tip control fungicide composition of the present invention is dissolved in 280 times water and sprayed onto the branches, leaves and Fruit.
  • the raw material dosage of the shoot control fungicide composition of the present invention is: 10 g of garlic, 10 g of ginger, 20 g of dianthus, 40 g of eucalyptus leaves, 300 g of red honeysuckle leaf, 30 g of purslane, and 0.01 g of meperium.
  • the preparation method of the tip control fungicide composition of the present invention includes the following steps:
  • 1Garlic processing technology peel the garlic, wash and mash it, enzymatically hydrolyze it at room temperature for 20 minutes, then add 60% ethanol by volume equivalent to 8 times the weight of the enzymolysis product, and ultrasonic wave at a constant temperature of 40 °C Auxiliary extraction for 60 minutes, filtering, centrifugation to take the supernatant under reduced pressure, concentration and drying to obtain garlic extract;
  • each microwave-assisted extraction process is as follows: microwave heating for 40 seconds, after naturally cooling to room temperature, heating is continued for 40 seconds, and then cooled to At room temperature, so cycle for 7 minutes;
  • Dianthus caryophylla extract can be obtained by concentration and drying under reduced pressure;
  • red glandular honeysuckle leaf extract Wash, dry and crush the red glandular honeysuckle leaf, then add 40% volumetric ethanol solution equivalent to 10 times the weight of red glandular honeysuckle leaf, and reflux 3 times at 70 °C , 2 hours each time, after the extracts are combined, concentrated under reduced pressure and dried to obtain the red glandular honeysuckle leaf extract;
  • step B Combine the crude powder of each extract in step B with 0.01g of mepazine, 9g of sodium lauryl ether sulfate, 2g of alkylphenol polyoxyethylene ether formaldehyde condensate sulfate, 2g of anhydrous ammonium sulfate, and 1g of polyoxypropylene glycerin Ether and 2g clay are mixed and evenly mixed;
  • step D After further pulverizing the mixture prepared in step C with a jet mill, add 2 g of vegetable gum, mix and stir evenly, and granulate with a granulator to prepare a water-dispersible granule.
  • the tip control fungicide composition of the present invention is used in the late spring and summer. When used, the tip control fungicide composition of the present invention is dissolved in 300 times the water and sprayed onto the branches, leaves and Fruit.
  • the raw material dosage of the shoot control fungicide composition of the present invention is: garlic 0.2g, ginger 0.2g, dianthus 2g, eucalyptus leaves 2g, erythrophylla honeysuckle leaves 300g, purslane 30g, meperium 0.3g.
  • the preparation method of the tip control fungicide composition of the present invention includes the following steps:
  • each microwave-assisted extraction process is as follows: microwave heating for 30 seconds, after naturally cooling to room temperature, heating is continued for 40 seconds, and then cooled to At room temperature, so cycle for 5 minutes;
  • Dianthus caryophylla extract can be obtained by concentration and drying under reduced pressure;
  • red glandular honeysuckle leaf extract wash, dry and crush the red glandular honeysuckle leaf, then add 70% volumetric ethanol solution equivalent to 12 times the weight of red glandular honeysuckle leaf, and reflux twice at 80 °C , 2 hours each time, after the extracts are combined, concentrated under reduced pressure and dried to obtain the red glandular honeysuckle leaf extract;
  • step B Combine the crude powder of each extract in step B with 0.3g of methylphenidate, 8g of fatty alcohol polyoxyethylene ether sulfonate, 3g of polyoxyethylene ether carboxylate, 2.5g of polyvinylpyrrolidone, 0.3g of emulsified silicone oil, 3.5 g Diatomaceous earth mixed and stirred evenly;
  • step D After further crushing the mixture prepared in step C with a jet mill, add 2 g of animal gum, mix and stir evenly, and then granulate with a granulator to prepare a water-dispersible granule.
  • the tip control fungicide composition of the present invention is used in late spring and summer. When used, the tip control fungicide composition of the present invention is dissolved in 200 times the water and sprayed onto the branches, leaves and Fruit.
  • Test method The sugar sugar orchard where the ulcer disease was more serious in previous years was selected as the test site. The experiment was set up with 5 treatments, with 3 replicates for each treatment, and 2 strains for each replicate for the test of sand sugar oranges.
  • the control fungicide prepared in Examples 1, 3, 5, 7, 8, and 10 was used as the test agent (the working solution was prepared according to the dilution factor described in the corresponding example), 20% thiazole zinc suspension 300 times, 400-fold solution and 500-fold solution were used as drug control, and clean water was used as blank control.
  • the first spraying was carried out when the summer shoots were about 2-3 cm, and then the second spraying was carried out at an interval of 10 days.
  • the relative control effect of the 20% thiazole zinc suspension 400 times solution is 2.34% and 9.9% higher than those obtained in Examples 1 and 10, respectively.
  • the obtained control fungicide has a good control effect on citrus ulcer disease.
  • the relative control effect of the 20% thiazole zinc suspension 500 times solution is 2.61% and 4.48% higher, respectively.
  • the difference between the formulations of Example 1 and Example 10 is only the content of mepazol, and they have a slight difference in the relative control effect. This may be due to the higher concentration of mepazol after the summer shoots. The more effective suppression of the hair growth and growth of the summer shoots makes the plant's nutrient supply relatively balanced and sufficient, and the plant's resistance has been enhanced.
  • Test method The sugar sugar orchard where the anthracnose was more severe last year was selected as the test site. Three treatments were set up in the experiment, and each treatment was repeated three times, and two plants were tested for sand sugar orange.
  • the control fungicide prepared in Examples 6 and 11 was used as the test agent (the working solution was prepared according to the dilution factor described in the corresponding example). Blank control.
  • the first spraying was carried out when the leaves of the spring shoots had not yet developed disease, and then the second spraying was carried out at an interval of 10 days.
  • spraying spray the entire plant evenly on the front and back sides, especially the new leaves must be sprayed in place, with the leaves completely wet and slightly dripping. No other chemical treatments will be carried out during the experiment, and the management measures are the same as conventional high-yield cultivation models.
  • Survey method Conduct a survey on prevention effects 15 days after the second spray. Each repetitive survey of 2 sand sugar oranges, each sugar sugar orange is sampled in five directions: east, west, south, north, and middle. Each direction randomly surveys 2 new shoots, and records all the leaves on the new shoots and records related data. Grading criteria for diseased leaf disease: level 0, disease-free; level 1, the diseased area accounts for less than 10% of the total leaf area; level 3, the diseased area accounts for 11-25% of the total leaf area; level 5, the diseased area It accounts for 26-40% of the total leaf area; at level 7, the lesion area accounts for 41-65% of the total leaf area; at level 9, the lesion area accounts for more than 65% of the total leaf area.
  • Test method Select sugar sugar oranges that have not been sprayed with any preservatives during the fruit-bearing period.
  • the experiment consists of 3 treatments, with 3 repeats for each treatment, with 50 sand oranges in each repeat.
  • the control fungicide prepared in Examples 3, 6, and 8 was used as the test agent (the working solution was prepared according to the dilution factor described in the corresponding example), and the 250g / L prochloramine 600 times solution was used as the agent control, without soaking.
  • the medicine is used as a blank control.
  • the infiltration method is used for the treatment, and the sugar oranges of different treatments are completely infiltrated in the corresponding chemical liquids of the treatment, and then picked up to dry after 1 minute.
  • each repeated fruit was packed into a plastic fruit box and placed completely randomly in a ventilated storage room at room temperature. After 3 days, single fruit bagging with film fruit bags. After 30, 45 and 60 days of storage, the incidence of penicillium citrus was investigated and recorded.
  • Investigation method record the incidence of fruit in each treatment and repeat, and calculate the disease rate and prevention effect according to the relevant data.
  • the calculation formula is as follows:
  • control fungicides obtained in Examples 6 and 8 and The control effectiveness of 250g / L prochloraz 600 times liquid has reached 100%; after 45 days of storage, compared with 250g / L prochloramine 600 times liquid, the controllable sterilization prepared in Examples 3, 6 and 8
  • the relative control effects of the agent treatments all declined to a certain extent, but the relative control effects of Example 6 and Example 8 still reached more than 90%; after 60 days of storage, the relative control effects of each treatment were 80.01%, 87.51%, 92.50% and 95.01%, of which the relative control effect of the control tip fungicide treatment prepared in Example 8 still reached more than 90%, although there is a certain difference from the 250g / L prochloramine 600 times solution, but the difference is not Big.
  • Test method Select the sugar sugar orange fruit tree with the same size, growth and no disease as the test plant.
  • the experiment adopts a split zone design, the spraying time is the main area, and the solution treatment is the secondary area: the spraying time (treatment) is divided into before and after the summer shoots.
  • the solution treatment in the first stage is the shoot control fungicide treatment (using the control prepared in Examples 1, 2, 4, 9, 11).
  • the tip fungicide is the test agent) and the water control.
  • the solution treatment in the second stage (the beginning of summer shoots) is the tip control fungicide treatment (prepared in Examples 1, 2, 5, 9, 12)
  • the control fungicide is the test agent) and water control.
  • Investigation methods (1) For plants that were treated with solution before summer shoots, take 10 representative spring shoots in each of the east, south, west, and north directions, and record the number of bud eye ripening and summer shoots. . After 10 days of treatment, randomly select 5 new shoots of summer shoots on each spring shoot to record their length and calculate the average value; Take 10 representative summer shoots randomly in each direction and mark them well. The length of each shoot was measured before treatment, and the length of the marked summer shoots was measured again 10 days after treatment.
  • Example 5 As can be seen from Table 5, at the beginning of Xia shoots, the tip control fungicides (Examples 5 and 9) containing higher concentrations of mepazone can effectively inhibit the growth of Xia shoots. The average elongation of summer shoots treated with shoot fungicides decreased by 60.3% and 64.7%, respectively. This shows that the tip control fungicides prepared in Example 5 and Example 9 have a good inhibitory effect on the summer shoots after hair pumping.
  • Test method The operation method is the same as that in Example 16, and the test agent is the control fungicide prepared in Examples 1, 2, 5, and 9;
  • Investigation method record the number of all young fruits of the plant to be tested at the time of treatment, and investigate the number of mature fruits at the time of harvest. The test results are shown in Table 6.

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Abstract

本发明公开了一种柑桔用控梢杀菌剂组合物，由以下重量份的原料制备而成：大蒜0.2-10份、生姜0.2-10份、石竹2-20份、桉树叶2-40份、红腺忍冬叶40-300份、马齿苋0.2-30份、甲哌鎓0.01-0.7份。通过将上述原料制备的活性成分与辅料混合，制成可湿性粉剂或水分散粒剂，可用于防治柑桔溃疡病、炭疽病、青霉病和绿霉病。在病害多发的春、夏两季，在兼具防治病害的同时，活性成分中的甲哌鎓还可以抑制柑桔春梢和夏梢的生长，达到化学控梢和促花保果的作用。本发明所述的控梢杀菌剂具有用量少、药效高、见效快、无残留的特点，使用起来既方便又安全。应用于柑桔生产中可起到稳产增产的作用。

Description

一种柑桔用控梢杀菌剂组合物及其制备方法 技术领域
本发明涉及农药技术领域，具体涉及一种柑桔用控梢杀菌剂组合物及其制备方法。
背景技术
柑桔溃疡病是一种世界性病害，此病起源于亚洲，且在亚洲国家发生最为普遍。其也是我国柑桔产区普遍的病害之一，在广东、广西、湖南等柑桔产区危害尤为严重。该病是一种细菌性病害，柑桔受害后在叶、枝、果上形成火山口状的病斑，大小2-8mm，后期造成落叶、落果，影响果实产量和品质。此病多发生在每年的4月上旬至11月下旬，主要为害春梢、夏梢和秋梢，以夏梢、秋梢受害最为严重，病菌可经气孔、皮孔及伤口侵染植株，在受侵染组织中迅速繁殖，刺激寄主细胞增大直至组织细胞肿胀破裂后死亡。目前，在生产上多使用化学制剂进行防治。一般于春梢展叶后7天左右和夏梢、秋梢萌芽后开始喷施铜制剂(如波尔多液、氧氯化铜、乙酸铜等)、抗菌素(如硫酸链霉素、金核霉素等)等杀菌剂，隔7-10天喷一次，共喷3次。
柑桔炭疽病是我国柑桔产区发生普遍、危害严重的病害之一，该病主要为害柑桔的叶片、枝梢、花和果实等器官，引起落叶、枯梢、落花、落果和烂果等，导致树势衰退，减产甚至绝收。该病是由炭疽菌引起的真菌性病害，经风雨或虫媒传播，由气孔、皮孔、伤口或者直接穿透表皮侵染植株组织。为了防治该病，生产上一般在落花后及落花后一个半月内在落花后及落花后一个半月内进行喷药，每隔10d左右喷1次，连续喷2～3次，在7、8月间再喷1次，以防落果。药剂可用40％灭病威500倍液，65％代森锌可湿性粉剂500倍液，70％甲基托布津可湿性粉剂800～1000倍液，50％多菌灵800倍液。
柑桔青霉病和绿霉病是柑桔采前和采后发生普遍、危害严重的病害，其主要为害果实，造成果实霉变、腐烂。该病主要是由青霉菌或绿霉菌引起的真菌性病害，通过孢子经伤口侵入柑桔果实。目前，除了改善采收和贮藏的条件外，主要还是依靠化学药剂对果实进行处理：可用双胍三辛烷基苯硫磺盐40％可湿性粉1000-2000倍液+万利得1000-2000倍液、70％甲基托布津可湿性粉剂或50％多菌灵可湿性粉剂500倍液。
但是，过分依赖化学杀菌剂对病害进行防治，容易造成病菌产生抗药性、农产品农残超标、环境污染等一系列负面影响。而利用植物天然提取物进行生物防治具有对环境友好、安全低残留、不容易导致抗药性产生等优点。已有研究表明，大蒜、生姜、石竹、桉树叶、红腺忍冬叶、马齿苋的提取物对金黄色葡萄球菌、大肠埃希菌、枯草芽孢杆菌等均具有抑制作用，部分植物提取物对供试菌的抑制效率甚至优于对照抗生素。因此，在柑桔种植生产中使用这些植物提取物的组合物作为杀菌剂也具有一定的应用前景。
在柑桔栽培过程中，控制夏梢的生长对于柑桔产量的形成具有至关重要的作用。在生产上采取的控梢技术有以肥控梢、人工控梢、以果控梢、以梢控梢和化学控梢等几种方式。其中，以肥控梢、以果控梢和以梢控梢由于操作要求高，效果不稳定，在生产上使用不普遍。人工控梢虽然操作简便、效果好，但是费时费力，且成本高，不太适合大规模种植的要求。而化学控梢以其见效快、操作简便、成本较低的优点而被越来越多的果农所接受。目前，用于化学控梢的药剂主要分为两大类：一类是以除草剂为主要成分的控梢剂，另一类是以植物生长调节剂为主要成分的控梢剂。前者虽然见效快，但药效短、易残留，且在结果期使用容易对果实外观造成影响，所以虽然有很多类似的专利产品，但在生产上鲜有使用。
植物生长调节剂类控梢剂以其安全、高效的特点，在生产上使用广泛，其中包括多效唑、矮壮素、甲哌嗡、乙烯利等。相对于其他几类植物生长调节剂，甲哌嗡的优点是药效温和、可以在花期使用。甲哌嗡又名缩节胺，是一种高效、低毒、低残留的植物生长调节剂。易被植物吸收，能抑制果树枝梢的萌发和生长。在春末和夏季时使用，可以减少因枝条大量萌发而造成的养分消耗，从而达到增加着果率，使果树稳产增产的作用。另外，使用甲哌嗡控梢，还可以避免由于人工摘梢造成的伤口，从而减少植株受病害侵染的机率。
发明内容
本发明是克服现有产品的不足，为柑桔栽培管理过程中提供一种安全、高效、环保，原料易获取、制备简便的控梢杀菌剂组合物及其制备方法。
为达到上述目的，本发明的技术方案为：
本发明的柑桔用控梢杀菌剂组合物，由包括以下重量份的原料制备而成：大蒜0.2-10份、生姜0.2-10份、石竹2-20份、桉树叶2-40份、红腺忍冬叶40-300 份、马齿苋0.2-30份、甲哌鎓0.01-0.7份。
进一步，所述的柑桔用控梢杀菌剂组合物，包括以下重量份的原料制备而成：大蒜2-5份、生姜2-8份、石竹4-10份、桉树叶10-30份、红腺忍冬叶50-260份、马齿苋2-25份、甲哌鎓0.02-0.6份。
进一步，所述的大蒜的加工工艺为：将大蒜去皮、洗净、捣碎，室温下室温下依靠大蒜自身含有的分解酶自然酶解20-40分钟，然后加入相当于酶解物2-6倍重量份的体积百分比为60-100％乙醇，在30-40℃恒温条件下超声波辅助提取60分钟以上，过滤，离心取上清液减压浓缩、烘干，即得大蒜提取物。
进一步，所述的生姜的加工工艺为：将生姜洗净、烘干、粉碎，然后加入相当于生姜4-8倍重量份的体积百分比为40-90％的乙醇，进行微波辅助萃取1-4次，然后过滤，加入与萃取溶液相同体积百分比的乙醇溶液进行洗涤，合并滤液和洗涤液减压浓缩、烘干即得生姜提取物；其中，每次微波辅助萃取过程如下：微波加热20-40秒，自然冷却至室温后，继续加热20-40秒，后再冷却至室温，如此循环3-7分钟。
进一步，所述的石竹的加工工艺为：将石竹烘干、粉碎，然后加入相当于石竹8-12倍重量份的体积百分比为60-100％的乙醇浸泡2-5天，每12小时搅拌1次，静置后过滤得粗提液；用8倍重量份的体积百分比为60-100％的乙醇浸提3小时，趁热过滤，然后用6倍重量份的体积百分比为60-100％的乙醇浸提2小时，趁热过滤，合并两次提取的滤液，进行减压浓缩、烘干即得石竹提取物。
进一步，所述的桉树叶的加工工艺为：将桉树叶洗净、烘干、粉碎，然后加入相当于桉树叶8-12倍重量份的体积百分比为60-100％的乙醇浸泡2-5天后，在20-40℃下超声波辅助提取10-30分钟，然后继续浸泡40-50小时，真空抽滤得提取液，减压浓缩，烘干后即得桉树叶提取物。
进一步，所述的红腺忍冬叶的加工工艺为：红腺忍冬叶洗净、烘干、粉碎，然后加入相当于红腺忍冬叶10-15倍重量份的体积百分比为40-90％的乙醇溶液，在70-85℃下回流1-3次，每次2小时，合并提取液后，减压浓缩、烘干即得红腺忍冬叶提取物。
进一步，所述的马齿苋的加工工艺为：将马齿苋洗净、烘干、粉碎，然后加入相当于马齿苋10-30倍重量份的体积百分比为40-90％的乙醇浸泡2-4天后，在 45-55℃下超声波辅助提取20-40分钟，然后继续浸泡20-30小时，真空抽滤得提取液，减压浓缩，烘干后即得马齿苋提取物。
进一步，所述的柑桔用控梢杀菌剂组合物与辅料混合，制成可湿性粉剂或水分散粒剂；
所述的辅料为润湿剂、分散剂、崩解剂、消泡剂、惰性填料、粘结剂中的一种或几种的混合物。
进一步，所述的润湿剂为十二烷基硫酸钠、烷基苯磺酸钠、木质素磺酸钠、月桂醇醚硫酸钠、脂肪醇聚氧乙烯醚磺酸钠、十二烷基硫酸钙、木质素磺酸钙中的一种或几种的混合物；
所述的分散剂为聚氧乙烯醚羧酸盐、聚氧乙烯醚磺酸盐、亚甲基双萘磺酸钠、木质素磺酸盐、萘磺酸甲醛缩合物钠盐、烷基酚聚氧乙烯醚甲醛缩合物硫酸盐、中的一种或几种的混合物；
所述的崩解剂为聚乙烯吡咯烷酮、无水硫酸铵、无水硫酸钠中的一种或几种的混合物；
所述的消泡剂为乳化硅油、高碳醇脂肪酸酯复合物、聚氧乙烯聚氧丙烯季戊四醇醚、聚氧乙烯聚氧丙醇胺醚、聚氧丙烯甘油醚、聚氧丙烯中的一种或几种的混合物；
所述的粘结剂为植物胶、动物胶、羟甲基纤维素钠、聚乙二醇中的一种或几种的混合物；
所述的惰性填料为硅藻土、陶土、高岭土、膨润土、凹凸棒土、白炭黑中的一种或几种的混合物。
进一步，所述的控梢杀菌剂组合物的制备方法包括以下步骤：
A、按重量份分别称取大蒜、生姜、石竹、桉树叶、红腺忍冬叶、马齿苋，分别将大蒜、生姜、石竹、桉树叶、红腺忍冬叶、马齿苋加工成大蒜提取物、生姜提取物、石竹提取物、桉树叶提取物、红腺忍冬提取物、马齿苋提取物；
B、将大蒜提取物、生姜提取物、石竹提取物、桉树叶提取物、红腺忍冬提取物、马齿苋提取物分别粉碎，得到相应的提取物粗粉；
C、将步骤B中的各提取物粗粉与甲哌嗡和除粘结剂以外的辅料混合搅拌均匀；
D、将步骤C中制备的混合物进一步粉碎，即得可湿性粉剂；
或者在可湿性粉剂的基础上，加入粘结剂，混合搅拌均匀后，进行造粒，即得水分散粒剂。
进一步，所述的控梢杀菌剂组合物，其使用方法为：在春末及夏季使用，使用时将本发明的控梢杀菌剂组合物溶于100-300倍水后，喷洒到植株的枝干、叶片和果实上即可。
针对此，本发明有以下显著效果：
本发明通过将多种植物源提取物按照一定的比例进行配伍，有效的发挥了各天然提取物的杀菌活性，有效的防治了柑桔溃疡病、炭疽病、青霉病、绿霉病，具有用量低、效果好、残留少的特点。另外，在防治病害的同时，本发明还可以起到控制枝梢生长的作用，有效抑制了柑桔春(末)梢和夏梢的生长，有利于柑桔的稳产高产。并且，一次施药既可以完成病害防治，又能实现对枝梢的化学调控，一举两得，省时、省工，节约成本。
具体实施方式
为了使本发明的目的、技术方案及优点更加简洁明了，本发明用以下具体实施例进行说明，但本发明绝非仅限于这些例子。以下所述仅为本发明较好的实施例，仅用于描述本发明，不能理解为对本发明的范围限制。应当指出的是，凡在本发明的精神和原则之内所做的任何修改、等同替换和改进等，均应包含在本发明的保护范围之内。
实施例1
本发明的控梢杀菌剂组合物的原料用量为：大蒜0.2g、生姜0.2g、石竹2g、桉树叶2g、红腺忍冬叶40g、马齿苋0.2g、甲哌鎓0.01g。
本发明的控梢杀菌剂组合物的制备方法包括以下步骤：
A、原料加工处理：
①大蒜的加工工艺为：将大蒜去皮、洗净、捣碎，室温下室温下依靠大蒜自身含有的分解酶自然酶解20分钟，然后加入相当于酶解物2倍重量的体积百分比为60％的乙醇，在30℃恒温条件下超声波辅助提取60分钟，过滤，离心取上清液减压浓缩、烘干，即得大蒜提取物；
②生姜的加工工艺为：将生姜洗净、烘干、粉碎，然后加入相当于生姜4 倍重量的体积百分比为40％的乙醇，进行微波辅助萃取1次，然后过滤，加入体积百分比为40％的乙醇溶液进行洗涤，合并滤液和洗涤液减压浓缩、烘干即得生姜提取物；其中，每次微波辅助萃取过程如下：微波加热20秒，自然冷却至室温后，继续加热20秒，后再冷却至室温，如此循环3分钟；
③石竹的加工工艺为：将石竹烘干、粉碎，然后加入相当于石竹8倍重量份的体积百分比为60％的乙醇浸泡2天，每12小时搅拌1次，静置后过滤得粗提液；用8倍重量的体积百分比为60％的乙醇浸提3小时，趁热过滤，然后用6倍重量的体积百分比为60％的乙醇浸提2小时，趁热过滤，合并两次提取的滤液，进行减压浓缩、烘干即得石竹提取物；
④桉树叶的加工工艺为：将桉树叶洗净、烘干、粉碎，然后加入相当于桉树叶8倍重量的体积百分比为60％的乙醇浸泡2天后，在20℃下超声波辅助提取10分钟，然后继续浸泡40小时，真空抽滤得提取液，减压浓缩，烘干后即得桉树叶提取物；
⑤红腺忍冬叶的加工工艺为：将红腺忍冬叶洗净、烘干、粉碎，然后加入相当于红腺忍冬叶10倍重量的体积百分比为40％的乙醇溶液，在70℃下回流1次，每次2小时，合并提取液后，减压浓缩、烘干即得红腺忍冬叶提取物；
⑥马齿苋的加工工艺为：将马齿苋全株洗净、烘干、粉碎，然后加入相当于马齿苋10倍重量的体积百分比为40％乙醇浸泡2天后，在45℃下超声波辅助提取20分钟，然后继续浸泡20小时，真空抽滤得提取液，减压浓缩、烘干后，即得马齿苋提取物；
B、将大蒜提取物、生姜提取物、石竹提取物、桉树叶提取物、红腺忍冬提取物、马齿苋提取物分别粉碎，得到相应的提取物粗粉；
C、将步骤B中各提取物粗粉与0.01g甲哌嗡、5g十二烷基硫酸钠、3g聚氧乙烯醚羧酸盐、0.5g乳化硅油、1g白炭黑混合搅拌均匀；
D、用气流粉碎机将步骤C中制备的混合物进一步粉碎即可制得可湿性粉剂。
本发明的控梢杀菌剂组合物，其使用方法为：在春末及夏季使用，使用时将本发明的控梢杀菌剂组合物溶于100倍水后，喷洒到植株的枝干、叶片和果实上。
实施例2
本发明的控梢杀菌剂组合物的原料用量为：大蒜0.5g、生姜0.5g、石竹3g、桉树叶5g、红腺忍冬叶50g、马齿苋1g、甲哌鎓0.02g。
本发明的控梢杀菌剂组合物的制备方法包括以下步骤：
A、原料加工处理：
①大蒜的加工工艺为：将大蒜去皮、洗净、捣碎，室温下室温下依靠大蒜自身含有的分解酶自然酶解22分钟，然后加入相当于酶解物3倍重量的体积百分比为65％的乙醇，在32℃恒温条件下超声波辅助提取65分钟，过滤，离心取上清液减压浓缩、烘干，即得大蒜提取物；
②生姜的加工工艺为：将生姜洗净、烘干、粉碎，然后加入相当于生姜5倍重量的体积百分比为45％的乙醇，进行微波辅助萃取2次；然后过滤，加入体积百分比为45％的乙醇溶液进行洗涤，合并滤液和洗涤液减压浓缩、烘干即得生姜提取物；其中，每次微波辅助萃取过程如下：微波加热25秒，自然冷却至室温后，继续加热25秒，后再冷却至室温，如此循环4分钟；
③石竹的加工工艺为：将石竹烘干、粉碎，然后加入相当于石竹9倍重量份的体积百分比为65％的乙醇浸泡3天，每12小时搅拌1次，静置后过滤得粗提液；用8倍重量的体积百分比为65％的乙醇浸提3小时，趁热过滤，然后用6倍重量的体积百分比为65％的乙醇浸提2小时，趁热过滤，合并两次提取的滤液，进行减压浓缩、烘干即得石竹提取物；
④桉树叶的加工工艺为：将桉树叶洗净、烘干、粉碎，然后加入相当于桉树叶9倍重量的体积百分比为65％的乙醇浸泡3天后，在22℃下超声波辅助提取12分钟，然后继续浸泡40小时，真空抽滤得提取液，减压浓缩，烘干后即得桉树叶提取物；
⑤红腺忍冬叶的加工工艺为：将红腺忍冬叶洗净、烘干、粉碎，然后加入相当于红腺忍冬叶11倍重量的体积百分比为45％的乙醇溶液，在72℃下回流2次，每次2小时，合并提取液后，减压浓缩、烘干即得红腺忍冬提取物；
⑥马齿苋的加工艺为：将马齿苋洗净、烘干、粉碎，然后加入相当于马齿笕12倍重量的体积百分比为45％的乙醇浸泡3天后，在46℃下超声波辅助提取22分钟，然后继续浸泡22小时，真空抽滤得提取液，减压浓缩，烘干后即得马齿苋提取物；
B、将大蒜提取物、生姜提取物、石竹提取物、桉树叶提取物、红腺忍冬提取物、马齿苋提取物分别粉碎，得到相应的提取物粗粉；
C、将步骤B中各提取物粗粉与0.02g甲哌嗡、4g烷基苯磺酸钠、3g聚氧乙烯醚磺酸盐、0.2g高碳醇脂肪酸酯复合物、2g凹凸棒土混合搅拌均匀；
D、用气流粉碎机将步骤C中制备的混合物进一步粉碎即可制得可湿性粉剂。
本发明的控梢杀菌剂组合物，其使用方法为：在春末及夏季使用，使用时将本发明的控梢杀菌剂组合物溶于120倍水后，喷洒到植株的枝干、叶片和果实上。
实施例3
本发明的控梢杀菌剂组合物的原料用量为：大蒜2g、生姜2g、石竹4g、桉树叶10g、红腺忍冬叶100g、马齿苋2g、甲哌鎓0.1g。
本发明的控梢杀菌剂组合物的制备方法包括以下步骤：
A、原料加工处理：
①大蒜的加工工艺：将大蒜去皮、洗净、捣碎，室温下自然酶解25分钟，然后加入相当于酶解物4倍重量的体积百分比为70％乙醇，在35℃恒温条件下超声波辅助提取70分钟，过滤，离心取上清液减压浓缩、烘干，即得大蒜提取物；
②生姜的加工工艺：将生姜洗净、烘干、粉碎，然后加入相当于生姜6倍重量的体积百分比为50％的乙醇，进行微波辅助萃取3次；然后过滤，加入体积百分比为50％的乙醇进行洗涤，合并滤液和洗涤液减压浓缩、烘干即得生姜提取物；其中，每次微波辅助萃取过程如下：微波加热30秒，自然冷却至室温后，继续加热30秒，后再冷却至室温，如此循环5分钟；
③石竹的加工工艺：将石竹烘干、粉碎，然后加入相当于石竹10倍重量的体积百分比为70％乙醇浸泡4天，每12小时搅拌1次，静置后过滤得粗提液；再依次用8倍重量的体积百分比为70％的乙醇浸提3小时，趁热过滤，然后用6倍重量的体积百分比为70％的乙醇浸提2小时，趁热过滤，合并两次提取的滤液，进行减压浓缩、烘干即得石竹提取液；
④桉树叶的加工工艺：将桉树叶洗净、烘干、粉碎，然后加入相当于桉树叶10倍重量的体积百分比为50％的乙醇浸泡4天后，在25℃下超声波辅助提取15 分钟，然后继续浸泡44小时，真空抽滤得提取液，减压浓缩，烘干后即得桉树叶提取物；
⑤红腺忍冬叶的加工工艺：将红腺忍冬叶洗净、烘干、粉碎，然后加入相当于红腺忍冬叶12倍重量的体积百分比为50％的乙醇溶液，在74℃下回流3次，每次2小时，合并提取液后，减压浓缩、烘干即得红腺忍冬叶提取物；
⑥马齿苋的加工工艺：将马齿苋全株洗净、烘干、粉碎，然后加入相当于马齿笕14倍重量的体积百分比为50％的乙醇浸泡4天后，在48℃下超声波辅助提取24分钟，然后继续浸泡24小时，真空抽滤得提取液，减压浓缩，烘干后即得马齿苋提取物；
B、将大蒜提取物、生姜提取物、石竹提取物、桉树叶提取物、红腺忍冬提取物、马齿苋提取物分别粉碎，得到相应的提取物粗粉；
C、将步骤B中各提取物粗粉与0.1g甲哌嗡、6g木质素磺酸纳、2.5g亚甲基双萘磺酸钠、0.1g聚氧乙烯聚氧丙烯季戊四醇醚、1.5g膨润土混合搅拌均匀；
D、用气流粉碎机将步骤C中制备的混合物进一步粉碎即可制得可湿性粉剂。
本发明的控梢杀菌剂组合物，其使用方法为：在春末及夏季使用，使用时将本发明的控梢杀菌剂组合物溶于140倍水后，喷洒到植株的枝干、叶片和果实上。
实施例4
本发明的控梢杀菌剂组合物的原料用量为：大蒜4g、生姜4g、石竹5g、桉树叶15g、红腺忍冬叶80g、马齿苋5g、甲哌鎓0.2g。
本发明的控梢杀菌剂组合物的制备方法包括以下步骤：
A、原料制备：
①大蒜的加工工艺：将大蒜去皮、洗净、捣碎，室温下自然酶解20分钟，然后加入相当于酶解物5倍重量的体积百分比为75％的乙醇，在35℃恒温条件下超声波辅助提取75分钟，过滤，在2800r/分钟下离心11分钟，取上清液减压浓缩、烘干，即得大蒜提取物；
②生姜的加工工艺：将生姜洗净、烘干、粉碎，然后加入相当于生姜7倍重量的体积百分比为75％的乙醇，进行微波辅助萃取4次；然后过滤，加入体积百分比为75％的乙醇进行洗涤，合并滤液和洗涤液减压浓缩、烘干即得生姜提取物； 其中，每次微波辅助萃取过程如下：微波加热28秒，自然冷却至室温后，继续加热28秒，后再冷却至室温，如此循环6分钟；
③石竹的加工工艺：将石竹烘干、粉碎，然后加入相当于石竹11倍重量的体积百分比为55％的乙醇浸泡5天，每12小时搅拌1次，静置后过滤得粗提液；再依次用8重量的体积百分比为75％的乙醇浸提3小时，趁热过滤，然后用6重量的体积百分比为75％的乙醇浸提2小时，趁热过滤，合并两次提取的滤液，进行减压浓缩、烘干即得石竹提取液；
④桉树叶的加工工艺：将桉树叶洗净、烘干、粉碎，然后加入相当于桉树叶11倍重量的体积百分比为75％的乙醇浸泡5天后，在26℃下超声波辅助提取16分钟，然后继续浸泡45小时，真空抽滤得提取液，减压浓缩烘干后即得桉树叶提取液；
⑤红腺忍冬叶的加工工艺：将红腺忍冬叶洗净、烘干、粉碎，然后加入相当于红腺忍冬叶14倍重量的体积百分比为55％的乙醇溶液，在76℃下回流1次，每次2小时，合并提取液后，减压浓缩、烘干即得红腺忍冬叶提取叶；
⑥马齿苋的加工工艺：将马齿苋全株洗净、烘干、粉碎，然后加入相当于马齿笕16倍重量的体积百分比为55％的乙醇浸泡2天后，在50℃下超声波辅助提取26分钟，然后继续浸泡25小时，真空抽滤得提取液，减压浓缩，烘干后即得马齿苋提取液。
B、将大蒜提取物、生姜提取物、石竹提取物、桉树叶提取物、红腺忍冬提取物、马齿苋提取物分别粉碎，得到相应的提取物粗粉；
C、将步骤B中各提取物粗粉与2g甲哌嗡、4g月桂醇醚硫酸钠、4g木质素磺酸盐、0.8g聚氧乙烯聚氧丙醇胺醚、3g高岭土混合搅拌均匀；
D、用气流粉碎机将步骤C中制备的混合物进一步粉碎即可制得可湿性粉剂。
本发明的控梢杀菌剂组合物，其使用方法为：在春末及夏季使用，使用时将本发明的控梢杀菌剂组合物溶于160倍水后，喷洒到植株的枝干、叶片和果实上。
实施例5
本发明的控梢杀菌剂组合物的原料用量为：大蒜5g、生姜8g、石竹10g、桉树叶20g、红腺忍冬叶100g、马齿苋10g、甲哌鎓0.3g。
本发明的控梢杀菌剂组合物的制备方法包括以下步骤：
A、原料制备：
①大蒜的加工工艺：将大蒜去皮、洗净、捣碎，室温下自然酶解30分钟，然后加入相当于酶解物6倍重量的体积百分比为80％乙醇，在36℃恒温条件下超声波辅助提取80分钟，过滤，离心取上清液减压浓缩、烘干，即得大蒜提取物；
②生姜的加工工艺：将生姜洗净、烘干、粉碎，然后加入相当于生姜8倍重量的体积百分比为60％乙醇，进行微波辅助萃取1次；然后过滤，加入体积百分比为75％的乙醇进行洗涤，合并滤液和洗涤液减压浓缩、烘干即得生姜提取物；其中，每次微波辅助萃取过程如下：微波加热30秒，自然冷却至室温后，继续加热30秒，后再冷却至室温，如此循环7分钟；
③石竹的加工工艺：将石竹烘干、粉碎，然后加入相当于石竹12倍重量的体积百分比为80％乙醇浸泡2天，每12小时搅拌1次，静置后过滤得粗提液；用8重量的体积百分比为80％的乙醇浸提3小时，趁热过滤，然后用6倍量80％的乙醇浸提2小时，趁热过滤，合并两次提取的滤液，进行减压浓缩、烘干即得；
④桉树叶的加工工艺：将桉树叶洗净、烘干、粉碎，然后加入相当于桉树叶12倍重量的体积百分比为80％乙醇浸泡2天后，在30℃下超声波辅助提取16分钟，然后继续浸泡46小时，真空抽滤得提取液，减压浓缩烘干后即得；
⑤红腺忍冬叶的加工工艺：将红腺忍冬叶洗净、烘干、粉碎，然后加入相当于红腺忍冬叶15倍重量份的体积百分比为60％乙醇溶液，在78℃下回流2次，每次2小时，合并提取液后，减压浓缩、烘干即得；
⑥马齿苋的加工工艺：将马齿苋洗净、烘干、粉碎，然后加入相当于马齿笕20倍重量的体积百分比为60％乙醇浸泡3天后，在51℃下超声波辅助提取30分钟，然后继续浸泡26小时，真空抽滤得提取液，减压浓缩烘干后即得
B、将大蒜提取物、生姜提取物、石竹提取物、桉树叶提取物、红腺忍冬提取物、马齿苋提取物分别粉碎，得到相应的提取物粗粉；
C、将步骤B中各提取物粗粉与0.3g甲哌嗡、8g脂肪醇聚氧乙烯醚磺酸钠、2g萘磺酸甲醛缩合物钠盐、1g聚氧丙烯甘油醚、2g陶土混合搅拌均匀；
D、用气流粉碎机将步骤C中制备的混合物进一步粉碎即可制得可湿性粉 剂。
本发明的控梢杀菌剂组合物，其使用方法为：在春末及夏季使用，使用时将本发明的控梢杀菌剂组合物溶于180倍水后，喷洒到植株的枝干、叶片和果实上。
实施例6
本发明的控梢杀菌剂组合物的原料用量为：大蒜7g、生姜8g、石竹15g、桉树叶30g、红腺忍冬叶200g、马齿苋20g、甲哌鎓0.4g。
本发明的控梢杀菌剂组合物的制备方法包括以下步骤：
A、原料制备：
①大蒜的加工工艺：将大蒜去皮、洗净、捣碎，室温下自然酶解27分钟，然后加入相当于酶解物2倍重量的体积百分比为85％乙醇，在38℃恒温条件下超声波辅助提取85分钟，过滤，离心取上清液减压浓缩、烘干，即得大蒜提取物；
②生姜的加工工艺：将生姜洗净、烘干、粉碎，然后加入相当于生姜4倍重量的体积百分比为70％乙醇，进行微波辅助萃取1次；然后过滤，加入体积百分比为75％的乙醇进行洗涤，合并滤液和洗涤液减压浓缩、烘干即得生姜提取物；其中，每次微波辅助萃取过程如下：微波加热35秒，自然冷却至室温后，继续加热35秒，后再冷却至室温，如此循环3分钟；
③石竹的加工工艺：将石竹烘干、粉碎，然后加入相当于石竹8倍重量的体积百分比为85％乙醇浸泡3天，每12小时搅拌1次，静置后过滤得粗提液；用8倍重量的体积百分比为85％的乙醇浸提3小时，趁热过滤，然后用和6重量的体积百分比为85％的乙醇浸提2小时，趁热过滤，合并两次提取的滤液，进行减压浓缩、烘干即得石竹提取物；
④桉树叶的加工工艺：将桉树叶洗净、烘干、粉碎，然后加入相当于桉树叶8倍重量的体积百分比为85％乙醇浸泡3天后，在32℃下超声波辅助提取22分钟，然后继续浸泡40小时，真空抽滤得提取液，减压浓缩烘干后即得桉树叶提取物；
⑤红腺忍冬叶的加工工艺：将红腺忍冬叶洗净、烘干、粉碎，然后加入相当于红腺忍冬叶10倍重量的体积百分比为70％的乙醇溶液，在82℃下回流3次，每次2小时，合并提取液后，减压浓缩、烘干即得红腺忍冬提取液；
⑥马齿苋的加工工艺：马齿苋洗净、烘干、粉碎，然后加入相当于马齿笕25倍重量的体积百分比为70％乙醇浸泡2天后，在53℃下超声波辅助提取32分钟，然后继续浸泡28小时，真空抽滤得提取液，减压浓缩烘干后即得马齿苋提取液；
B、将大蒜提取物、生姜提取物、石竹提取物、桉树叶提取物、红腺忍冬提取物、马齿苋提取物分别粉碎，得到相应的提取物粗粉；
C、将步骤B中各提取物粗粉与0.4g甲哌嗡、7g十二烷基硫酸钙、2g烷基酚聚氧乙烯醚甲醛缩合物硫酸盐、0.5g聚氧丙烯、1g硅藻土混合搅拌均匀；
D、用气流粉碎机将步骤C中制备的混合物进一步粉碎即可制得可湿性粉剂。
本发明的控梢杀菌剂组合物，其使用方法为：在春末及夏季使用，使用时将本发明的控梢杀菌剂组合物溶于200倍水后，喷洒到植株的枝干、叶片和果实上。
实施例7
本发明的控梢杀菌剂组合物的原料用量为：大蒜8g、生姜9g、石竹18g、桉树叶35g、红腺忍冬叶260g、马齿苋25g、甲哌鎓0.5g。
本发明的控梢杀菌剂组合物的制备方法包括以下步骤：
A、原料制备：
①大蒜的加工工艺：将大蒜去皮、洗净、捣碎，室温下自然酶解29分钟，然后加入相当于酶解物4倍重量的体积百分比为95％乙醇，在39℃恒温条件下超声波辅助提取90分钟，过滤，离心取上清液减压浓缩、烘干，即得大蒜提取物；
②生姜的加工工艺：将生姜洗净、烘干、粉碎，然后加入相当于生姜6加入80％乙醇，进行微波辅助萃取2次；然后过滤，加入体积百分比为80％的乙醇进行洗涤，合并滤液和洗涤液减压浓缩、烘干即得生姜提取物；其中，每次微波辅助萃取过程如下：微波加热38秒，自然冷却至室温后，继续加热38秒，后再冷却至室温，如此循环4分钟；
③石竹的加工工艺：将石竹烘干、粉碎，然后加入相当于石竹10倍重量的体积百分比为95％的乙醇浸泡3天，每12小时搅拌1次，静置后过滤得粗提液；用8重量的体积百分比为90％的乙醇浸提3小时，趁热过滤，然后用6倍重量的 体积百分比为90％的乙醇浸提2小时，趁热过滤，合并两次提取的滤液，进行减压浓缩、烘干即得石竹提取物；
④桉树叶的加工工艺：将桉树叶洗净、烘干、粉碎，然后加入相当于桉树叶10倍重量的体积百分比为90％的乙醇浸泡4天后，在35℃下超声波辅助提取28分钟，然后继续浸泡49小时，真空抽滤得提取液，减压浓缩烘干后即得桉树叶提取物；
⑤红腺忍冬叶的加工工艺：将红腺忍冬叶洗净、烘干、粉碎，然后加入相当于红腺忍冬叶12倍重量的体积百分比为80％的乙醇溶液，在83℃下回流1次，每次2小时，合并提取液后，减压浓缩、烘干即得红腺忍冬也提取物；
⑥马齿苋的加工工艺：将马齿苋洗净、烘干、粉碎，然后加入相当于马齿笕28倍重量的体积百分比为80％乙醇浸泡3天后，在54℃下超声波辅助提取38分钟，然后继续浸泡28小时，真空抽滤得提取液，减压浓缩烘干后即得马齿苋提取物；
B、将大蒜提取物、生姜提取物、石竹提取物、桉树叶提取物、红腺忍冬提取物、马齿苋提取物分别粉碎，得到相应的提取物粗粉；
C、将步骤B中各提取物粗粉与0.5g甲哌嗡、6g木质素磺酸钙、4g聚氧乙烯醚羧酸盐、1.5g聚乙烯吡咯烷酮、0.3g乳化硅油、1g白炭黑混合搅拌均匀；
D、用气流粉碎机将步骤C中制备的混合物进一步粉碎后，加入0.8g植物胶胶，混合搅拌均匀后，用造粒机进行造粒，即可制得水分散粒剂。
本发明的控梢杀菌剂组合物，其使用方法为：在春末及夏季使用，使用时将本发明的控梢杀菌剂组合物溶于220倍水后，喷洒到植株的枝干、叶片和果实上。
实施例8
本发明的控梢杀菌剂组合物的原料用量为：大蒜10g、生姜10g、石竹20g、桉树叶40g、红腺忍冬叶300g、马齿苋30g、甲哌鎓0.6g。
本发明的控梢杀菌剂组合物的制备方法包括以下步骤：
A、原料制备：
①大蒜的加工工艺：将大蒜去皮、洗净、捣碎，室温下自然酶解40分钟，然后加入相当于酶解物6倍重量的体积百分比为95％乙醇，在40℃恒温条件下超声波辅助提取100分钟，过滤，离心取上清液减压浓缩、烘干，即得大蒜提取 物；
②生姜的加工工艺：将生姜洗净、烘干、粉碎，然后加入相当于生姜8倍重量的体积百分比为90％乙醇，进行微波辅助萃取3次；然后过滤，加入体积百分比为90％的乙醇进行洗涤，合并滤液和洗涤液减压浓缩、烘干即得生姜提取物；其中，每次微波辅助萃取过程如下：微波加热40秒，自然冷却至室温后，继续加热40秒，后再冷却至室温，如此循环7分钟；
③石竹的加工工艺：将石竹烘干、粉碎，然后加入相当于石竹12倍重量的体积百分比为98％乙醇浸泡5天，每12小时搅拌1次，静置后过滤得粗提液；再依次用8倍重量的体积百分比为100％的乙醇浸提3小时，趁热过滤，然后用6倍重量的体积百分比为100％的乙醇浸提2小时，趁热过滤，合并两次提取的滤液，进行减压浓缩、烘干即得石竹提取物；
④桉树叶的加工工艺：将桉树叶洗净、烘干、粉碎，然后加入相当于桉树叶12倍重量的体积百分比为98％的乙醇浸泡5天后，在40℃下超声波辅助提取30分钟，然后继续浸泡50小时，真空抽滤得提取液，减压浓缩烘干后即得桉树叶提取物；
⑤红腺忍冬叶的加工工艺：将红腺忍冬叶洗净、烘干、粉碎，然后加入相当于红腺忍冬叶15倍重量的体积百分比为90％的乙醇溶液，在85℃下回流3次，每次2小时，合并提取液后，减压浓缩、烘干即得红腺忍冬叶提取物；
⑥马齿苋的加工工艺：将马齿苋洗净、烘干、粉碎，然后加入相当于马齿笕30倍重量的体积百分比为90％的乙醇浸泡4天后，在55℃下超声波辅助提取40分钟，然后继续浸泡30小时，真空抽滤得提取液，减压浓缩烘干后即得马齿苋提取物；
B、将大蒜提取物、生姜提取物、石竹提取物、桉树叶提取物、红腺忍冬提取物、马齿苋提取物分别粉碎，得到相应的提取物粗粉；
C、将步骤B中各提取物粗粉与0.6g甲哌嗡、4g十二烷基硫酸钠、3g聚氧乙烯醚磺酸盐、2.5g无水硫酸铵、0.6g高碳醇脂肪酸酯复合物、1.5g凹凸棒土混合搅拌均匀；
D、用气流粉碎机将步骤C中制备的混合物进一步粉碎后，加入1g动物胶，混合搅拌均匀后，用造粒机进行造粒，即可制得水分散粒剂。
本发明的控梢杀菌剂组合物，其使用方法为：在春末及夏季使用，使用时将本发明的控梢杀菌剂组合物溶于240倍水后，喷洒到植株的枝干、叶片和果实上。
实施例9
本发明的控梢杀菌剂组合物的原料用量为：大蒜10g、生姜10g、石竹20g、桉树叶40g、红腺忍冬叶300g、马齿苋30g、甲哌鎓0.7g。
本发明的控梢杀菌剂组合物的制备方法包括以下步骤：
A、原料制备：
①大蒜的加工工艺：将大蒜去皮、洗净、捣碎，室温下自然酶解40分钟，然后加入相当于酶解物6倍重量的体积百分比为95％乙醇，在40℃恒温条件下超声波辅助提取100分钟，过滤，离心取上清液减压浓缩、烘干，即得大蒜提取物；
②生姜的加工工艺：将生姜洗净、烘干、粉碎，然后加入相当于生姜8倍重量的体积百分比为90％乙醇，进行微波辅助萃取3次；然后过滤，加入体积百分比为90％的乙醇进行洗涤，合并滤液和洗涤液减压浓缩、烘干即得生姜提取物；其中，每次微波辅助萃取过程如下：微波加热40秒，自然冷却至室温后，继续加热40秒，后再冷却至室温，如此循环7分钟；
③石竹的加工工艺：将石竹烘干、粉碎，然后加入相当于石竹12倍重量的体积百分比为98％乙醇浸泡5天，每12小时搅拌1次，静置后过滤得粗提液；再依次用8倍重量的体积百分比为100％的乙醇浸提3小时，趁热过滤，然后用6倍重量的体积百分比为100％的乙醇浸提2小时，趁热过滤，合并两次提取的滤液，进行减压浓缩、烘干即得石竹提取物；
④桉树叶的加工工艺：将桉树叶洗净、烘干、粉碎，然后加入相当于桉树叶12倍重量的体积百分比为98％的乙醇浸泡5天后，在40℃下超声波辅助提取30分钟，然后继续浸泡50小时，真空抽滤得提取液，减压浓缩烘干后即得桉树叶提取物；
⑤红腺忍冬叶的加工工艺：将红腺忍冬叶洗净、烘干、粉碎，然后加入相当于红腺忍冬叶15倍重量的体积百分比为90％的乙醇溶液，在85℃下回流3次，每次2小时，合并提取液后，减压浓缩、烘干即得红腺忍冬叶提取物；
⑥马齿苋的加工工艺：将马齿苋洗净、烘干、粉碎，然后加入相当于马齿笕 30倍重量的体积百分比为90％的乙醇浸泡4天后，在55℃下超声波辅助提取40分钟，然后继续浸泡30小时，真空抽滤得提取液，减压浓缩烘干后即得马齿苋提取物；
B、将大蒜提取物、生姜提取物、石竹提取物、桉树叶提取物、红腺忍冬提取物、马齿苋提取物分别粉碎，得到相应的提取物粗粉；
C、将步骤B中各提取物粗粉与0.7g甲哌嗡、5g烷基苯磺酸钠、4g亚甲基双萘磺酸钠、2g无水硫酸钠、0.2g聚氧乙烯聚氧丙烯季戊四醇醚、2g膨润土混合搅拌均匀；
D、用气流粉碎机将步骤C中制备的混合物进一步粉碎后，加入2g羧甲基纤维素钠，混合搅拌均匀后，用造粒机进行造粒，即可制得水分散粒剂。
本发明的控梢杀菌剂组合物，其使用方法为：在春末及夏季使用，使用时将本发明的控梢杀菌剂组合物溶于260倍水后，喷洒到植株的枝干、叶片和果实上。
实施例10
本发明的控梢杀菌剂组合物的原料用量为：大蒜0.2g、生姜0.2g、石竹2g、桉树叶2g、红腺忍冬叶40g、马齿苋0.2g、甲哌鎓0.7g。
本发明的控梢杀菌剂组合物的制备方法包括以下步骤：
A、原料制备：
①大蒜的加工工艺：将大蒜去皮、洗净、捣碎，室温下自然酶解20分钟，然后加入相当于酶解物6倍重量的体积百分比为100％乙醇，在30℃恒温条件下超声波辅助提取70分钟，过滤，离心取上清液减压浓缩、烘干，即得大蒜提取物；
②生姜的加工工艺：将生姜洗净、烘干、粉碎，然后加入相当于生姜8倍重量的体积百分比为90％乙醇，进行微波辅助萃取2次；然后过滤，加入体积百分比为90％的乙醇进行洗涤，合并滤液和洗涤液减压浓缩、烘干即得生姜提取物；其中，每次微波辅助萃取过程如下：微波加热20秒，自然冷却至室温后，继续加热20秒，后再冷却至室温，如此循环4分钟；
③石竹的加工工艺：将石竹烘干、粉碎，然后加入相当于石竹8倍重量的体积百分比为100％乙醇浸泡2天，每12小时搅拌1次，静置后过滤得粗提液；再依次用8倍重量的体积百分比为100％的乙醇浸提3小时，趁热过滤，然后用6 倍重量的体积百分比为100％的乙醇浸提2小时，趁热过滤，合并两次提取的滤液，进行减压浓缩、烘干即得石竹提取物；
④桉树叶的加工工艺：将桉树叶洗净、烘干、粉碎，然后加入相当于桉树叶10倍重量的体积百分比为100％的乙醇浸泡2天后，在20℃下超声波辅助提取20分钟，然后继续浸泡40小时，真空抽滤得提取液，减压浓缩烘干后即得桉树叶提取物；
⑤红腺忍冬叶的加工工艺：将红腺忍冬叶洗净、烘干、粉碎，然后加入相当于红腺忍冬叶13倍重量的体积百分比为90％的乙醇溶液，在75℃下回流2次，每次2小时，合并提取液后，减压浓缩、烘干即得红腺忍冬叶提取物；
⑥马齿苋的加工工艺：将马齿苋洗净、烘干、粉碎，然后加入相当于马齿笕30倍重量的体积百分比为90％的乙醇浸泡2天后，在45℃下超声波辅助提取30分钟，然后继续浸泡25小时，真空抽滤得提取液，减压浓缩烘干后即得马齿苋提取物；
B、将大蒜提取物、生姜提取物、石竹提取物、桉树叶提取物、红腺忍冬提取物、马齿苋提取物分别粉碎，得到相应的提取物粗粉；
C、将步骤B中各提取物粗粉与0.7g甲哌嗡、3g木质素磺酸钠、3g萘磺酸甲醛缩合物钠盐、2g无水硫酸钠、1g聚氧乙烯聚氧丙醇胺醚、3g高岭土混合搅拌均匀；
D、用气流粉碎机将步骤C中制备的混合物进一步粉碎后，加入2.5g聚乙二醇，混合搅拌均匀后，用造粒机进行造粒，即可制得水分散粒剂。
本发明的控梢杀菌剂组合物，其使用方法为：在春末及夏季使用，使用时将本发明的控梢杀菌剂组合物溶于280倍水后，喷洒到植株的枝干、叶片和果实上。
实施例11
本发明的控梢杀菌剂组合物的原料用量为：大蒜10g、生姜10g、石竹20g、桉树叶40g、红腺忍冬叶300g、马齿苋30g、甲哌鎓0.01g。
本发明的控梢杀菌剂组合物的制备方法包括以下步骤：
A、原料制备：
①大蒜的加工工艺：将大蒜去皮、洗净、捣碎，室温下自然酶解20分钟，然后加入相当于酶解物8倍重量的体积百分比为60％乙醇，在40℃恒温条件下 超声波辅助提取60分钟，过滤，离心取上清液减压浓缩、烘干，即得大蒜提取物；
②生姜的加工工艺：将生姜洗净、烘干、粉碎，然后加入相当于生姜8倍重量的体积百分比为40％乙醇，进行微波辅助萃取1次；然后过滤，加入体积百分比为40％的乙醇进行洗涤，合并滤液和洗涤液减压浓缩、烘干即得生姜提取物；其中，每次微波辅助萃取过程如下：微波加热40秒，自然冷却至室温后，继续加热40秒，后再冷却至室温，如此循环7分钟；
③石竹的加工工艺：将石竹烘干、粉碎，然后加入相当于石竹12倍重量的体积百分比为60％乙醇浸泡2天，每12小时搅拌1次，静置后过滤得粗提液；再依次用8倍重量的体积百分比为60％的乙醇浸提3小时，趁热过滤，然后用6倍重量的体积百分比为60％的乙醇浸提2小时，趁热过滤，合并两次提取的滤液，进行减压浓缩、烘干即得石竹提取物；
④桉树叶的加工工艺：将桉树叶洗净、烘干、粉碎，然后加入相当于桉树叶8倍重量的体积百分比为60％的乙醇浸泡5天后，在20℃下超声波辅助提取30分钟，然后继续浸泡50小时，真空抽滤得提取液，减压浓缩烘干后即得桉树叶提取物；
⑤红腺忍冬叶的加工工艺：将红腺忍冬叶洗净、烘干、粉碎，然后加入相当于红腺忍冬叶10倍重量的体积百分比为40％的乙醇溶液，在70℃下回流3次，每次2小时，合并提取液后，减压浓缩、烘干即得红腺忍冬叶提取物；
⑥马齿苋的加工工艺：将马齿苋洗净、烘干、粉碎，然后加入相当于马齿笕30倍重量的体积百分比为40％的乙醇浸泡3天后，在55℃下超声波辅助提取20分钟，然后继续浸泡30小时，真空抽滤得提取液，减压浓缩烘干后即得马齿苋提取物；
B、将大蒜提取物、生姜提取物、石竹提取物、桉树叶提取物、红腺忍冬提取物、马齿苋提取物分别粉碎，得到相应的提取物粗粉；
C、将步骤B中各提取物粗粉与0.01g甲哌嗡、9g月桂醇醚硫酸钠、2g烷基酚聚氧乙烯醚甲醛缩合物硫酸盐、2g无水硫酸铵、1g聚氧丙烯甘油醚、2g陶土混合搅拌均匀；
D、用气流粉碎机将步骤C中制备的混合物进一步粉碎后，加入2g植物胶， 混合搅拌均匀后，用造粒机进行造粒，即可制得水分散粒剂。
本发明的控梢杀菌剂组合物，其使用方法为：在春末及夏季使用，使用时将本发明的控梢杀菌剂组合物溶于300倍水后，喷洒到植株的枝干、叶片和果实上。
实施例12
本发明的控梢杀菌剂组合物的原料用量为：大蒜0.2g、生姜0.2g、石竹2g、桉树叶2g、红腺忍冬叶300g、马齿苋30g、甲哌鎓0.3g。
本发明的控梢杀菌剂组合物的制备方法包括以下步骤：
A、原料制备：
①大蒜的加工工艺：将大蒜去皮、洗净、捣碎，依靠大蒜自身含有的分解酶自然酶解30分钟，然后加入相当于酶解物4倍重量的体积百分比为80％乙醇，在35℃恒温条件下超声波辅助提取70分钟，过滤，离心取上清液减压浓缩、烘干，即得大蒜提取物；
②生姜的加工工艺：将生姜洗净、烘干、粉碎，然后加入相当于生姜6倍重量的体积百分比为60％乙醇，进行微波辅助萃取1次；然后过滤，加入体积百分比为60％的乙醇进行洗涤，合并滤液和洗涤液减压浓缩、烘干即得生姜提取物；其中，每次微波辅助萃取过程如下：微波加热30秒，自然冷却至室温后，继续加热40秒，后再冷却至室温，如此循环5分钟；
③石竹的加工工艺：将石竹烘干、粉碎，然后加入相当于石竹10倍重量的体积百分比为80％乙醇浸泡4天，每12小时搅拌1次，静置后过滤得粗提液；再依次用8倍重量的体积百分比为80％的乙醇浸提3小时，趁热过滤，然后用6倍重量的体积百分比为80％的乙醇浸提2小时，趁热过滤，合并两次提取的滤液，进行减压浓缩、烘干即得石竹提取物；
④桉树叶的加工工艺：将桉树叶洗净、烘干、粉碎，然后加入相当于桉树叶10倍重量的体积百分比为80％的乙醇浸泡3天后，在30℃下超声波辅助提取20分钟，然后继续浸泡45小时，真空抽滤得提取液，减压浓缩烘干后即得桉树叶提取物；
⑤红腺忍冬叶的加工工艺：将红腺忍冬叶洗净、烘干、粉碎，然后加入相当于红腺忍冬叶12倍重量的体积百分比为70％的乙醇溶液，在80℃下回流2次，每次2小时，合并提取液后，减压浓缩、烘干即得红腺忍冬叶提取物；
⑥马齿苋的加工工艺：将马齿苋洗净、烘干、粉碎，然后加入相当于马齿笕25倍重量的体积百分比为70％的乙醇浸泡3天后，在50℃下超声波辅助提取30分钟，然后继续浸泡25小时，真空抽滤得提取液，减压浓缩烘干后即得马齿苋提取物；
B、将大蒜提取物、生姜提取物、石竹提取物、桉树叶提取物、红腺忍冬提取物、马齿苋提取物分别粉碎，得到相应的提取物粗粉；
C、将步骤B中各提取物粗粉与0.3g甲哌嗡、8g脂肪醇聚氧乙烯醚磺酸钠、3g聚氧乙烯醚羧酸盐、2.5g聚乙烯吡咯烷酮、0.3g乳化硅油、3.5g硅藻土混合搅拌均匀；
D、用气流粉碎机将步骤C中制备的混合物进一步粉碎后，加入2g动物胶，混合搅拌均匀后，用造粒机进行造粒，即可制得水分散粒剂。
本发明的控梢杀菌剂组合物，其使用方法为：在春末及夏季使用，使用时将本发明的控梢杀菌剂组合物溶于200倍水后，喷洒到植株的枝干、叶片和果实上。
实施例13 对柑桔溃疡病的药效实验
试验方法：选择往年溃疡病发生较为严重的沙糖桔园作为试验地点。试验设5个处理，每个处理3个重复，每个重复2株供试沙糖桔。以实施例1、3、5、7、8、10中制得的控梢杀菌剂作为试验药剂(按照相应实施例中说明的稀释倍数配制工作液)，20％噻唑锌悬浮剂300倍液、400倍液和500倍液作为药剂对照，清水作为空白对照。于夏梢抽出2-3cm左右时进行第一次喷药，之后间隔10天再进行第二次喷药。喷药时对全株正反面均匀喷雾，特别是新叶一定要喷施到位，以叶片完全湿润轻微滴水为度。试验期间不再进行其他药剂处理，管理措施同常规高产栽培模式。
调查方法：第一次喷药前进行病情基数调查，供试植株并未表现出感染溃疡病的症状。第二次喷药后15天进行防效调查。每个重复调查2棵沙糖桔，每株沙糖桔按东、西、南、北、中5个方向取样，每个方向随机调查2个新梢，并记录新梢上的所有树叶数、病叶数和病叶相应的发病情况。病叶发病情况分级标准：0级，无病斑；1级，每叶1-5个病斑；3级，每叶6-10个病斑；5级，每叶11-15个病斑；7级，每叶16-20个病斑；9级，每叶21个以上病斑。
病情指数与防效计算方法：
病情指数＝Σ(各级病叶数×相对级数值)/(调查总叶数×9)×100
防效(％)＝(空白对照病情指数－施药处理病情指数)/空白对照病情指数×100
试验结果如表1所示。经观察，施药期间柑桔叶片生长正常，未出现明显药害症状，表明本发明所述控梢杀菌剂在供试剂量范围内对柑桔安全。
表1药剂处理对柑桔溃疡病的防治效果
Figure PCTCN2019100729-appb-000001
结果与分析：由表1可知，实施例1、3、5、7、8、10中制得的控梢杀菌剂的相对防效分别为51.17％、61.49％、69.05％、77.85％、80.47％和53.04％，20％噻唑锌悬浮剂300倍液、400倍液和500倍液的相对防效分别为71.39％、59.15％和48.56％。实施例7、8中所得药剂的相对防效比20％噻唑锌悬浮剂300倍液的相对防效分别高出6.46％和9.08％；实施例3、5中所得药剂的相对防效比这表明，实施例8中所得控梢杀菌剂对柑桔溃疡病具有较好的防治效果20％噻唑锌悬浮剂400倍液的相对防效分别高出2.34％和9.9％；实施例1、10中所得所得控梢杀菌剂对柑桔溃疡病具有较好的防治效果20％噻唑锌悬浮剂500倍液的相对防效分别高出2.61％和4.48％。实施例1与实施例10在配方上的区别仅在于甲哌嗡的含量，而它们在相对防效上有微小的差别，这可能是由于夏梢抽发后，较高浓度的甲哌嗡能够更有效的抑制夏梢的抽发和生长，使得植株的养分供给相对较为均衡、充足，植株的抵抗力有所增强所形成的差异。
实施例14 对柑桔炭疽病的药效实验
试验方法：选择上一年炭疽病发生较为严重的沙糖桔园作为试验地点。试验设3个处理，每个处理3个重复，每个重复2株供试沙糖桔。以实施例6、11中制得的控梢杀菌剂作为试验药剂(按照相应实施例中说明的稀释倍数配制工作液)，80％代森锰锌可湿性粉剂600倍液作为药剂对照，清水作为空白对照。于4月中旬春梢叶片尚未发病时进行第一次喷药，之后间隔10天再进行第二次喷药。喷药时对全株正反面均匀喷雾，特别是新叶一定要喷施到位，以叶片完全湿润轻微滴水为度。试验期间不再进行其他药剂处理，管理措施同常规高产栽培模式。
调查方法：第二次喷药后15天进行防效调查。每个重复调查2棵沙糖桔，每株沙糖桔按东、西、南、北、中5个方向取样，每个方向随机调查2个新梢，并记录新梢上的全部叶片并记录相关数据。病叶发病情况分级标准：0级，无病；1级，病斑面积占全叶面积的10％以下；3级，病斑面积占全叶面积的11-25％；5级，病斑面积占全叶面积的26-40％；7级，病斑面积占全叶面积的41-65％；9级，病斑面积占全叶面积的65％以上。
病情指数与防效计算方法：
病情指数＝Σ(各级病叶数×相对级数值)/(调查总叶数×9)×100
防效(％)＝(空白对照病情指数－施药处理病情指数)/空白对照病情指数×100
试验结果如表2所示。
表2药剂处理对柑桔炭疽病的防治效果
Figure PCTCN2019100729-appb-000002
结果与分析：由表2可知，实施例6、11中制得的控梢杀菌剂的相对防效分别为80.66％和，80％代森锰锌可湿性粉剂600倍液的相对防效为79.52％。由此可知，实施例6和实施例11中制得的控梢杀菌剂的防效略高于对照药剂(80％代森锰锌可湿性粉剂)。试验结果表明实施例6和实施例11中所得控梢杀菌剂对柑桔溃疡病具有较好的防治效果。另外，经观察，药剂处理期间叶片未出现明显 药害，表明药剂对沙糖桔生长安全。
实施例15 对柑桔青霉病、绿霉病的药效实验
试验方法：选择挂果期未喷施过任何保鲜剂的沙糖桔备用。试验设3个处理，每个处理3个重复，每个重复中有50个沙糖桔。以实施例3、6、8中制得的控梢杀菌剂作为试验药剂(按照相应实施例中说明的稀释倍数配制工作液)，250g/L咪鲜胺乳油600倍液作为药剂对照，不浸药的作为空白对照。处理采用侵渍法，将不同处理的沙糖桔分别完全侵渍于该处理对应的药液中，1分钟后捞起晾干。侵渍后每个重复的果实装进塑料果箱中，并完全随机地放置于通风贮藏房间内，常温贮藏。3天后用薄膜果袋单果套袋。贮藏30、45和60天后分别调查记录柑桔青霉病的发病情况。
调查方法：记录各处理各重复内的果实发病情况，并根据相关数据计算出病果率和防效。计算公式如下所示：
病果率(％)＝病果数/处理总果数×100
防效(％)＝(对照区病果率-处理区病果率)/对照区病果率×100
试验结果如表3所示。
表3药剂处理对柑桔青霉病、绿霉病的防治效果
Figure PCTCN2019100729-appb-000003
Figure PCTCN2019100729-appb-000004
结果与分析：由表3可知，通过在贮藏前使用药剂浸果，可以有效的降低青霉病和绿霉病对果实的影响。贮藏30天后，实施例3、6、8中制得的控梢杀菌剂对青霉病、绿霉病均有较好的防效，其中实施例6和实施例8中所得控梢杀菌剂与250g/L咪鲜胺乳油600倍液的防效均达到了100％；贮藏45天后，相比250g/L咪鲜胺乳油600倍液，实施例3、6、8中制得的控梢杀菌剂处理的相对防效均有一定的下降，但实施例6和实施例8的相对防效任然达到了90％以上；贮藏60天后，各处理的相对防效分别为80.01％、87.51％、92.50％和95.01％，其中实施例8中制得的控梢杀菌剂处理的相对防效任然达到了90％以上，与250g/L咪鲜胺乳油600倍液虽有一定差异，但相差不大。这说明实施例3、6、8中制得的控梢杀菌剂对柑桔青霉病和绿霉病具有较好的防治效果，且实施例8中制得的控梢杀菌剂的防效更持久。
实施例16 控梢效果实验
试验方法：选择大小、长势一致、无病害的沙糖桔果树作为供试植株。试验采用裂区设计，喷施时间为主区，溶液处理为副区：喷施时间(处理)分为夏梢抽发前和夏梢抽发初期。每个主区内设置两个溶液处理，第一阶段(夏梢抽发前)内的溶液处理分别是控梢杀菌剂处理(以实施例1、2、4、9、11中制得的控梢杀菌剂为供试药剂)和清水对照，第二阶段(夏梢抽发初期)内的溶液处理分别是控梢杀菌剂处理(以实施例1、2、5、9、12中制得的控梢杀菌剂为供试药剂)和清水对照。每个溶液处理设置3个重复，每个重复3株沙糖桔。
调查方法：(1)夏梢抽发前进行溶液处理的植株，在其东、南、西、北四个方向各取10枝有代表性的春梢，记录其芽眼熟和夏梢抽发数。处理10天后，在每个春梢上随机选择5枝新发夏梢记录其长度，并计算均值；(2)夏梢抽发初期进行溶液处理的植株，在植株东、南、西、北四个方向上随机各取10枝有代表性的夏梢，并做好标记。在处理前测量每枝夏梢的长度，处理10天后再次测量已标记的夏梢的长度。
试验结果如表4、表5所示。
表4夏梢抽发前进行药剂处理对柑桔夏梢生长的抑制效果
药剂 春梢芽眼数 夏梢抽发数 夏梢抽发率(％) 夏梢平均长度(cm)
实施例1 70 5 7.1 7.2
实施例2 78 3 3.8 5.7
实施例4 85 2 2.4 3.9
实施例9 90 2 2.22 3.3
实施例11 66 5 7.6 7.0
空白对照 81 9 11.1 10.6
表5夏梢抽发初期进行药剂处理对柑桔夏梢生长的抑制效果
药剂 处理前平梢长(cm) 处理后平均梢长(cm) 夏梢平均伸长量(cm)
实施例1 5.1 16.4 11.3
实施例2 5.9 15.3 9.4
实施例5 6.3 11.7 5.4
实施例9 5.5 10.3 4.8
实施例12 6.7 17.3 10.6
空白对照 7.0 20.6 13.6
结果分析：(1)由表4可知，在夏梢抽发前使用实施例1、2、4、9、11中制得的控梢杀菌剂均能减少夏梢的抽发数量，其中实施例2、4、9处理的效果优于实施例1和实施例12，但实施例2、4、9之间相差不大。这就说明，在夏梢抽发之前，只需要低浓度的甲哌嗡即可达到较好的控梢效果。
(2)由表5可知，夏梢抽发初期，含较高浓度甲哌嗡的控梢杀菌剂(实施例5、实施例9)能够有效的抑制夏梢的生长，与对照相比，控梢杀菌剂处理的夏梢平均伸长量分别减少了60.3％和64.7％。这表明实施例5和实施例9中制得的控梢杀菌剂对抽发后的夏梢有良好的抑制作用。
实施例17 稳产(增产)效果实验
试验方法：操作方法同实施例16，供试试剂为实施例1、2、5、9中制得的控梢杀菌剂；
调查方法：处理时记录供试植株的全部幼果数，采收时调查成熟果数。试验结果如表6所示。
表6控梢杀菌剂处理对柑桔产量的影响
Figure PCTCN2019100729-appb-000005
结果与分析：由表6可知，实施例1、2、5、9中制得的控梢杀菌剂能够有效的增加着果率，且夏梢抽发前喷施控梢杀菌剂的处理，其着果率略高于夏梢抽发初期的处理。这可能是夏梢抽发前喷施控梢杀菌剂，减少了夏梢的抽发数量，减少了养分的消耗，使得植株有更多的养分供给果实生长。控梢杀菌剂处理的单果重较之清水对照略有降低，这可能是由于着果率增加，单株果数增加，植株在营养供给上相对不足导致的。但是，从单株产量上看，控梢杀菌剂处理的植株还是优于对照的。

Claims (11)

  1. 一种柑桔用控梢杀菌剂组合物，其特征在于，由包括以下重量份的原料制备而成：大蒜0.2-10份、生姜0.2-10份、石竹2-20份、桉树叶2-40份、红腺忍冬叶40-300份、马齿苋0.2-30份、甲哌鎓0.01-0.7份。
  2. 如权利要求1所述的柑桔用控梢杀菌剂组合物，其特征在于，由包括以下重量份的原料制备而成：大蒜2-5份、生姜2-8份、石竹4-10份、桉树叶10-30份、红腺忍冬叶50-260份、马齿苋2-25份、甲哌鎓0.02-0.6份。
  3. 如权利要求1或2所述的柑桔用控梢杀菌剂组合物，其特征在于，所述的大蒜的加工工艺为：将大蒜去皮、洗净、捣碎，室温下依靠大蒜自身含有的分解酶自然酶解20-40分钟，然后加入相当于酶解物2-6倍重量的体积百分比为60-100％的乙醇，在30-40℃恒温条件下超声波辅助提取60分钟以上，过滤，离心取上清液减压浓缩、烘干，即得大蒜提取物。
  4. 如权利要求1或2所述的柑桔用控梢杀菌剂组合物，其特征在于，所述的生姜的加工工艺为：将生姜洗净、烘干、粉碎，然后加入相当于生姜4-8倍重量的体积百分比为40-90％的乙醇，进行微波辅助萃取1-4次；然后过滤，加入与萃取溶液相同体积百分比的乙醇溶液进行洗涤，合并滤液和洗涤液减压浓缩、烘干即得生姜提取物；
    其中，每次微波辅助萃取过程如下：微波加热20-40秒，自然冷却至室温后，继续加热20-40秒，后再冷却至室温，如此循环3-7分钟。
  5. 如权利要求1或2所述的柑桔用控梢杀菌剂组合物，其特征在于，所述的石竹的加工工艺为：将石竹烘干、粉碎，然后加入相当于石竹8-12倍重量的体积百分比为60-100％的乙醇浸泡2-5天，每12小时搅拌1次，静置后过滤得粗提液；用8倍重量的体积百分比为60-100％的乙醇浸提3小时，趁热过滤，然后用6倍重量的体积百分比为60-100％的乙醇浸提2小时，趁热过滤，合并两次提取的滤液，进行减压浓缩、烘干即得石竹提取物。
  6. 如权利要求1或2所述柑桔用控梢杀菌剂组合物，其特征在于，所述的桉树叶的加工工艺为：将桉树叶洗净、烘干、粉碎，然后加入相当于桉树叶8-12 倍重量的体积百分比为60-100％的乙醇浸泡2-5天后，在20-40℃下超声波辅助提取10-30分钟，然后继续浸泡40-50小时，真空抽滤得提取液，减压浓缩，烘干后即得桉树叶提取物。
  7. 如权利要求1或2所述柑桔用控梢杀菌剂组合物，其特征在于，所述的红腺忍冬叶的加工工艺为：将红腺忍冬叶洗净、烘干、粉碎，然后加入相当于红腺忍冬叶10-15倍重量的体积百分比为40-90％的乙醇溶液，在70-85℃下回流1-3次，每次2小时，合并提取液后，减压浓缩、烘干即得红腺忍冬叶提取物。
  8. 如权利要求1或2所述的柑桔用控梢杀菌剂组合物，其特征在于，所述的马齿苋的加工工艺为：将马齿苋全株洗净、烘干、粉碎，然后加入相当于马齿笕10-30倍重量的体积百分比为40-90％的乙醇浸泡2-4天后，在45-55℃下超声波辅助提取20-40分钟，然后继续浸泡20-30小时，真空抽滤得提取液，减压浓缩，烘干后即得马齿苋提取物。
  9. 如权利要求1-8任一项所述的柑桔用控梢杀菌剂组合物与辅料混合，制成可湿性粉剂或水分散粒剂，其特征在于：
    所述的辅料为润湿剂、分散剂、崩解剂、消泡剂、惰性填料、粘结剂中的一种或几种的混合物。
  10. 如权利要求9所述的柑桔用控梢杀菌剂组合物，其特征在于：
    所述的润湿剂为十二烷基硫酸钠、烷基苯磺酸钠、木质素磺酸钠、月桂醇醚硫酸钠、脂肪醇聚氧乙烯醚磺酸钠、十二烷基硫酸钙、木质素磺酸钙中的一种或几种的混合物；
    所述的分散剂为聚氧乙烯醚羧酸盐、聚氧乙烯醚磺酸盐、亚甲基双萘磺酸钠、木质素磺酸盐、萘磺酸甲醛缩合物钠盐、烷基酚聚氧乙烯醚甲醛缩合物硫酸盐、中的一种或几种的混合物；
    所述的崩解剂为聚乙烯吡咯烷酮、无水硫酸铵、无水硫酸钠中的一种或几种的混合物；
    所述的消泡剂为乳化硅油、高碳醇脂肪酸酯复合物、聚氧乙烯聚氧丙烯季戊四醇醚、聚氧乙烯聚氧丙醇胺醚、聚氧丙烯甘油醚、聚氧丙烯中的一种或几种的混合物；
    所述的粘结剂为植物胶、动物胶、羟甲基纤维素钠、聚乙二醇中的一种或几 种的混合物；
    所述的惰性填料为硅藻土、陶土、高岭土、膨润土、凹凸棒土、白炭黑中的一种或几种的混合物。
  11. 如权利要求10所述的柑桔用控梢杀菌剂组合物，其特征在于，其制备方法包括以下步骤：
    A、按重量份分别称取大蒜、生姜、石竹、桉树叶、红腺忍冬叶、马齿苋，分别将大蒜、生姜、石竹、桉树叶、红腺忍冬叶、马齿苋加工成大蒜提取物、生姜提取物、石竹提取物、桉树叶提取物、红腺忍冬提取物、马齿苋提取物；
    B、将大蒜提取物、生姜提取物、石竹提取物、桉树叶提取物、红腺忍冬提取物、马齿苋提取物分别粉碎，得到相应的提取物粗粉；
    C、将步骤B中的各提取物粗粉与甲哌嗡和除粘结剂外的辅料混合搅拌均匀；
    D、将步骤C中制备的混合物进一步粉碎，即得可湿性粉剂；
    或者在可湿性粉剂的基础上，加入粘结剂，混合搅拌均匀后，进行造粒，即得水分散粒剂。
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