TW201909743A - Oil-based concentrate, preparation method thereof and use thereof - Google Patents

Oil-based concentrate, preparation method thereof and use thereof Download PDF

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TW201909743A
TW201909743A TW107127925A TW107127925A TW201909743A TW 201909743 A TW201909743 A TW 201909743A TW 107127925 A TW107127925 A TW 107127925A TW 107127925 A TW107127925 A TW 107127925A TW 201909743 A TW201909743 A TW 201909743A
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吳一凡
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大陸商江蘇龍燈化學有限公司
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    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
    • A01N25/00Biocides, 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
    • A01N25/02Biocides, 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 containing liquids as carriers, diluents or solvents
    • A01N25/04Dispersions, emulsions, suspoemulsions, suspension concentrates or gels
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
    • A01N25/00Biocides, 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
    • A01N25/30Biocides, 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 characterised by the surfactants
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
    • A01N43/00Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/34Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom
    • A01N43/40Biocides, 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
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
    • A01N47/00Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid
    • A01N47/02Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid the carbon atom having no bond to a nitrogen atom
    • A01N47/06Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid the carbon atom having no bond to a nitrogen atom containing —O—CO—O— groups; Thio analogues thereof

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  • Life Sciences & Earth Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Wood Science & Technology (AREA)
  • Environmental Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Dentistry (AREA)
  • Pest Control & Pesticides (AREA)
  • Agronomy & Crop Science (AREA)
  • Zoology (AREA)
  • Plant Pathology (AREA)
  • Toxicology (AREA)
  • Chemical & Material Sciences (AREA)
  • Dispersion Chemistry (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)
  • Medicinal Preparation (AREA)
  • Cosmetics (AREA)

Abstract

Disclosed are an oil-based concentrate, a preparation method therefor and the use thereof, the oil-based concentrate comprises the following components: a component a: at least one spirotetramat active substance which is solid at room temperature; a component b: at least one pyriproxyfen active substance which is solid at room temperature; a component c: at least one fatty acid ester with general formula R1-COO-R2 and/or R1-COO-R2-OOC-R1; a component d: at least one non-ionic surfactant and/or at least one anionic surfactant; and optionally a component e: one or at least two additives selected from an emulsifier, a defoaming agent, a preservative, an antioxidant, a colourant or an inert filling material; wherein the pyriproxyfen is dissolved in a molecular state in the component c, and the spirotetramat is suspended in a particle state in the component c. The oil-based concentrate prepared by the present invention can effectively resolve the problem of particle size increase of spirotetramat during storage, improve the stability of a preparation, and enhance the compounding effect and the bioavailability.

Description

油基濃縮液,其製備方法和其用途Oil-based concentrated liquid, preparation method and application thereof

本發明屬於農藥領域,涉及一種油基濃縮液及其製備方法和用途。The invention belongs to the field of pesticides and relates to an oil-based concentrated liquid and a preparation method and application thereof.

賜派滅(spirotetramat)是拜耳公司開發的季酮酸類化合物,是迄今具有雙向內吸傳導性能的現代殺蟲劑之一。該化合物可以在整個植物體內向上向下移動,抵達葉面和樹皮,從而防治如生菜和白菜內葉上及果樹皮上的害蟲。這種獨特的內吸性能可以保護新生莖、葉和根部,防止害蟲的卵和幼蟲生長。其另一個特點是持效期長,可提供長達8周的有效防治。Spirotetramat is a quaternary ketone acid compound developed by Bayer, and it is one of the modern insecticides that have two-way systemic conductance to date. The compound can move up and down throughout the plant to reach foliage and bark, thus controlling pests such as lettuce and cabbage on the inner leaves and fruit bark. This unique systemic ability protects new stems, leaves and roots from the growth of pest eggs and larvae. Another feature is the long duration of effect, which can provide effective control for up to 8 weeks.

百利普芬(pyriproxyfen)是苯醚類擾亂昆蟲生長的昆蟲生長調節劑,屬保幼激素類似物的新型殺蟲劑,具有內吸轉移活性、低毒,持效期長,對作物安全,對魚類低毒,對生態環境影響小的特點。對梨木虱、煙粉虱、介殼蟲、小菜蛾、甜菜夜蛾、斜紋夜蛾、梨黃木虱和薊馬等有良好的防治效果,同時本品對蒼蠅、蚊蟲等衛生害蟲具有很好的防治效果。具有抑制蚊、蠅幼蟲化蛹和羽化作用。蚊、蠅幼蟲接觸該藥劑,基本上都在蛹期死亡,不能羽化。該藥劑持效期長達1個月左右,且使用方便,無異味,是較好的滅蚊、蠅藥物。Pyriproxyfen is a phenyl ether insect growth regulator that disturbs the growth of insects. It is a new type of insecticide with juvenile hormone analogs. It has systemic transfer activity, low toxicity, long duration, and is safe for crops. Low toxicity to fish and small impact on the ecological environment. It has a good control effect on Psylla, Bemisia tabaci, scale insects, Plutella xylostella, Spodoptera exigua, Spodoptera litura, Psylla Psylla and Thrips, etc. At the same time, this product has a good control effect on health pests such as flies and mosquito . It can inhibit mosquito and fly larva pupation and emergence. Mosquito and fly larvae basically die in the pupal stage when they contact the agent and cannot emerge. The duration of the drug is about 1 month, and it is easy to use and has no odor. It is a good mosquito and fly medicine.

目前關於賜派滅與百利普芬複配的製劑專利也有報導,CN103283787A公開了賜派滅與百利普芬複配組合,同時提及製備複配的劑型包括可濕性粉劑、水分散粒劑、懸浮劑、懸乳劑、水乳劑、微乳劑和微囊懸浮劑。可實際製備過程中以上劑型或多或少都會遇到困難。比如因為百利普芬原藥熔點為45-47℃,製備可濕性粉劑、水分散粒劑或懸浮劑都會因為熔點太低不適合或者無法加工,且以上製劑製備出的產品都會在54℃熱貯下因原藥熔化而導致產品失敗,理論上不可行。製備成微囊懸浮劑、微膠囊懸浮劑-懸浮劑雖然理論上是可行的,但因為微膠囊技術複雜,對加工設備要求高、成本高,而不被研發人員採用。製備成水乳劑、微乳劑雖然技術相對簡單成熟、成本低,但該方法受限於賜派滅與百利普芬的溶解性和溶解度,很難製備高含量的複配製劑,尤其是含量總和大於30%的複配製劑,且或多或少用到對環境不友好的溶劑而被市場所淘汰。At present, there is also a report on the formulation of Ciparam and Paliprofen. CN103283787A discloses the combination of Ciparam and Paliprofen. It also mentions that the formulation of the formulation includes wettable powder, water-dispersible granule Agents, suspensions, suspoemulsions, aqueous emulsions, microemulsions and microcapsule suspensions. The above dosage forms may encounter more or less difficulties in the actual preparation process. For example, because the melting point of the original drug of Beliperfin is 45-47 ° C, the preparation of wettable powders, water-dispersible granules or suspensions will not be suitable or cannot be processed because the melting point is too low, and the products prepared by the above formulations will be heated at 54 ° C Product failure due to melting of the original drug is not theoretically feasible. Although it is theoretically feasible to prepare the microcapsule suspension agent and the microcapsule suspension agent-suspending agent, because the microcapsule technology is complicated, it requires high processing equipment and high cost, so it is not used by the R & D personnel. Although the technology for preparing aqueous emulsions and microemulsions is relatively simple and mature, and the cost is low, this method is limited by the solubility and solubility of Cipamir and Paliprofen, and it is difficult to prepare high-content complex preparations, especially the sum of the contents. More than 30% of the formulations, and more or less use of environmentally unfriendly solvents were eliminated by the market.

因此,目前市場上迫切需要研製出環境友好,粒徑和劑型穩定,加工工藝簡單,製備成本低的優良製劑。Therefore, there is an urgent need on the market to develop excellent formulations that are environmentally friendly, stable in particle size and dosage form, simple in processing technology, and low in preparation cost.

針對現有技術的不足,本發明的目的在於提供一種油基濃縮液及其製備方法和用途。In view of the shortcomings of the prior art, an object of the present invention is to provide an oil-based concentrated liquid, and a preparation method and application thereof.

為達此目的,本發明採用以下技術方案: 一方面,本發明提供一種油基濃縮液,所述油基濃縮液包括如下組分: a 組分:至少一種室溫下為固體的賜派滅活性物; b 組分:至少一種室溫下為固體的百利普芬活性物; c 組分:至少一種具有通式R1 -COO-R2 和/或R1 -COO-R2 -OOC-R1 脂肪酸酯,其中R1 為具有10~25個碳原子的烷基和/或烯基,R2 為具有1~10個碳原子的烷基; d 組分:至少一種非離子表面活性劑和/或至少一種陰離子表面活性劑; 任選地 e 組分:一種或至少兩種選自乳化劑、消泡劑、防腐劑、抗氧化劑、著色劑或惰性填充材料的添加劑; 其中百利普芬是以分子狀態溶解於c組分中,賜派滅是以顆粒狀態懸浮於c組分中。To achieve this, the present invention adopts the following technical solutions: In one aspect, the present invention provides an oil-based concentrate, which includes the following components: a component: at least one kind of solid-state at room temperature Actives; component b: at least one belipofen active that is solid at room temperature; component c: at least one having the general formula R 1 -COO-R 2 and / or R 1 -COO-R 2 -OOC -R 1 fatty acid ester, wherein R 1 is an alkyl group and / or alkenyl group having 10 to 25 carbon atoms, and R 2 is an alkyl group having 1 to 10 carbon atoms; d component: at least one non-ionic surface Active agent and / or at least one anionic surfactant; optionally e component: one or at least two additives selected from emulsifiers, defoamers, preservatives, antioxidants, colorants or inert filler materials; Ripfen is dissolved in the c component in a molecular state, and Cipafil is suspended in the c component in a particulate state.

在本發明中,通過對油基濃縮液的組分進行特定選擇搭配,尤其是使用脂肪酸酯成分,使得油基濃縮液能有效的控制賜派滅在儲存過程中粒徑增長問題,大大抑制了賜派滅懸浮顆粒的粒徑增長,提高了製劑的穩定性,提升了賜派滅的作用效果,同時百利普芬能以分子狀態穩定的存在於濃縮液中,不會有晶體析出,兩者活性物之間互不影響,保持各自的狀態於濃縮物中,增強了複配效果。In the present invention, by specifically selecting and matching the components of the oil-based concentrated liquid, especially the use of fatty acid ester components, the oil-based concentrated liquid can effectively control the problem of particle size growth during storage and greatly inhibit In order to increase the particle size of Cipaim, the stability of the formulation is improved, and the effect of Cipaim is improved. At the same time, Paliprofen can exist in the concentrated solution in a stable molecular state without crystal precipitation. The two actives do not affect each other, and maintain their respective states in the concentrate, which enhances the compounding effect.

在本發明中,在賜派滅與百利普芬進行複配的油基濃縮液中,不含增稠劑(例如植物油或礦物油),但卻能夠表現出優異的穩定性,提高了含有賜派滅 和百利普芬活性物製劑的穩定性。In the present invention, the oil-based concentrated liquid compounded by Papex and Paliprofen does not contain a thickener (such as vegetable oil or mineral oil), but it can show excellent stability and improve its content. Contains Papex and the stability of the active ingredient formulation of belipurin.

在本發明中,所述油基濃縮物單個組分的含量可在較寬的範圍內。In the present invention, the content of the individual components of the oil-based concentrate may be in a wide range.

較佳地,所述油基濃縮液包括如下重量百分比的組分:0.1~30%的所述a組分、0.1~30%的所述b組分、20~90%的所述c組分、1~30%的所述d組分和0~40%的所述e組分;Preferably, the oil-based concentrated liquid includes the following components in weight percentages: 0.1 to 30% of the a component, 0.1 to 30% of the b component, and 20 to 90% of the c component 1 to 30% of the d component and 0 to 40% of the e component;

在本發明中,通過特定用量的各組分相互配合,使得油基濃縮液的組分間達到較佳的配合狀態,有效的控制賜派滅在儲存過程中粒徑增長問題,抑制賜派滅懸浮顆粒的粒徑增長,提高製劑的穩定性。In the present invention, the components of a specific amount of each other are matched to each other, so that the components of the oil-based concentrated liquid can achieve a better coordination state, effectively control the particle size increase problem during storage, and inhibit the suspension The particle size increases and the stability of the formulation is improved.

較佳地,所述賜派滅與百利普芬重量配比為1:10~10:1,例如1:1、1:2、1:3、1:4、1:5、1:6、1:7、1:8、1:9、1:10、2:1、3:1、4:1、5:1、6:1、7:1、8:1、9:1或10:1,較佳為1:5~5:1。Preferably, the weight ratio of Ciparam to Paliprofen is 1: 10 ~ 10: 1, such as 1: 1, 1: 2, 1: 3, 1: 4, 1: 5, 1: 6. , 1: 7, 1: 8, 1: 9, 1:10, 2: 1, 3: 1, 4: 1, 5: 1, 6: 1, 7: 1, 8: 1, 9: 1 or 10 : 1, preferably 1: 5 ~ 5: 1.

在本發明中,當所述賜派滅與百利普芬重量配比為1:10~10:1時,兩者可以各自保持更加優良的活性,以各自的狀態存在於濃縮液中,能夠產生良好的複配效果。In the present invention, when the weight ratio of Cipafil and Paliprofen is 1: 10 ~ 10: 1, both of them can maintain more excellent activity, exist in the concentrated liquid in their respective states, and can Produce good compounding effect.

本發明中,所述油基濃縮液能完全溶解百利普芬,使百利普芬以分子狀態存在,並且能夠使賜派滅顆粒懸浮。所述c組分較佳為通式R1 -COO-R2 和/或R1 -COO-R2 -OOC-R1 脂肪酸酯。其中R1 為具有10至25個碳原子的直鏈或支鏈烷基和/或烯基,R2 為具有1-10個碳原子的直鏈或支鏈烷基。符合上述結構的脂肪酸酯通常為C1 -C10 烷基的一元醇或二元醇與脂肪酸形成的C10 -C25 的脂肪酸酯。所述的C1 -C10 烷基的一元醇或二元醇可以是乙醇、丙醇、丁醇、戊醇、己醇、乙二醇、丙二醇、丁二醇、戊二醇或己二醇等。所述的脂肪酸較佳為具有偶數個碳原子的脂肪酸,例如可以是葵酸、芥酸、月桂酸、豆蔻酸、棕櫚酸、硬脂酸、油酸、亞油酸、亞麻油酸或花生酸等。In the present invention, the oil-based concentrated solution can completely dissolve beliprefin, make beliprefin exist in a molecular state, and be able to suspend ciprofen particles. The c component is preferably a fatty acid ester of the general formula R 1 -COO-R 2 and / or R 1 -COO-R 2 -OOC-R 1 . Wherein R 1 is a straight or branched chain alkyl and / or alkenyl group having 10 to 25 carbon atoms, and R 2 is a straight or branched chain alkyl group having 1 to 10 carbon atoms. The fatty acid ester conforming to the above structure is usually a C 10 -C 25 fatty acid ester of a mono- or diol of a C 1 -C 10 alkyl group and a fatty acid. The C 1 -C 10 alkyl mono- or diol may be ethanol, propanol, butanol, pentanol, hexanol, ethylene glycol, propylene glycol, butanediol, pentanediol or hexanediol Wait. The fatty acid is preferably a fatty acid having an even number of carbon atoms. For example, the fatty acid may be acetic acid, erucic acid, lauric acid, myristic acid, palmitic acid, stearic acid, oleic acid, linoleic acid, linoleic acid, or arachidic acid. Wait.

較佳地,所述c組分中R1 為具有12~20個碳原子的烷基和/或烯基,例如12、13、14、15、16、17、18、19或20碳原子,進一步較佳為具有12~18個碳原子的烷基和/或烯基;R2 為具有2~8個碳原子的烷基,例如2、3、4、5、6、7或8個碳原子,進一步較佳為具有2~6個碳原子的烷基。Preferably, R 1 in the c component is an alkyl and / or alkenyl group having 12 to 20 carbon atoms, for example, 12, 13, 14, 15, 16, 17, 18, 19 or 20 carbon atoms, Further preferred are alkyl and / or alkenyl groups having 12 to 18 carbon atoms; R 2 is an alkyl group having 2 to 8 carbon atoms, such as 2, 3, 4, 5, 6, 7, or 8 carbons The atom is more preferably an alkyl group having 2 to 6 carbon atoms.

較佳地,所述烷基為直鏈烷基或支鏈烷基。Preferably, the alkyl group is a linear alkyl group or a branched alkyl group.

較佳地,所述c組分為油酸乙酯、油酸丁酯、月桂酸己酯、棕櫚酸乙二酯或亞油酸戊二酯中的任意一種或至少兩種的組合。Preferably, the component c is any one or a combination of at least two of ethyl oleate, butyl oleate, hexyl laurate, ethylene palmitate, or gluteryl linoleate.

在本發明中,上述脂肪酸酯或其組合能夠調節油基濃縮液的穩定性,能夠有效抑制賜派滅在儲存過程中粒徑的增長。In the present invention, the above-mentioned fatty acid ester or a combination thereof can regulate the stability of the oil-based concentrated liquid, and can effectively suppress the increase of the particle size of Ciproxil during storage.

較佳地,所述非離子表面活性劑選自甲基丙烯酸與甲基丙烯酸酯的共聚物、脂肪醇與環氧乙烷和/或環氧丙烷的聚合物、環氧乙烷-環氧丙烷嵌段共聚物、脂肪醇聚氧乙烯醚、烷基糖苷、聚乙烯醇、聚乙烯吡咯烷酮、烷基乙氧基化物、烷基芳基乙氧基化物或吐溫中的任意一種或至少兩種的組合。Preferably, the non-ionic surfactant is selected from the group consisting of a copolymer of methacrylic acid and methacrylate, a polymer of fatty alcohol and ethylene oxide and / or propylene oxide, and ethylene oxide-propylene oxide Any one or at least two of block copolymer, fatty alcohol polyoxyethylene ether, alkyl glycoside, polyvinyl alcohol, polyvinyl pyrrolidone, alkyl ethoxylate, alkyl aryl ethoxylate or Tween The combination.

在本發明中,所述非離子表面活性劑具有分散、乳化和增溶等作用。In the present invention, the non-ionic surfactant has the functions of dispersing, emulsifying and solubilizing.

較佳地,所述陰離子表面活性劑選自木質素磺酸鹽(Borresperse NA)、琥珀酸磺酸鹽、萘磺酸鹽甲醛縮聚物、三苯乙烯乙氧基化物的硫酸鹽、三苯乙烯乙氧基化物的磷酸鹽或聚羧酸鹽中的任意一種或至少兩種的組合。Preferably, the anionic surfactant is selected from the group consisting of Borresperse NA, succinate sulfonate, naphthalene sulfonate formaldehyde polycondensate, sulfate of tristyrene ethoxylate, and tristyrene. Any one or a combination of at least two of ethoxylate phosphate or polycarboxylate.

在本發明中,所述陰離子表面活性劑具有澄清淨化作用。In the present invention, the anionic surfactant has a clarifying and purifying effect.

在本發明中,所述油基濃縮液中a組分的重量百分比為0.1~30%,例如0.1%、0.8%、2%、5%、6.9%、8.4%、9.6%、11%、12.9%、15%、17%、18%、19.5%、21.2%、25%、27.5%或30%,較佳為5~20%。In the present invention, the weight percentage of the component a in the oil-based concentrated solution is 0.1 to 30%, for example, 0.1%, 0.8%, 2%, 5%, 6.9%, 8.4%, 9.6%, 11%, 12.9 %, 15%, 17%, 18%, 19.5%, 21.2%, 25%, 27.5% or 30%, preferably 5-20%.

在本發明中,所述油基濃縮液中b組分的重量百分比為0.1~30%,例如0.1%、0.8%、2%、5%、6.9%、8.4%、9.6%、11%、12.9%、15%、17%、18%、19.5%、21.2%、25%、27.5%或30%,較佳為5~20%。In the present invention, the weight percentage of component b in the oil-based concentrated solution is 0.1-30%, for example, 0.1%, 0.8%, 2%, 5%, 6.9%, 8.4%, 9.6%, 11%, 12.9 %, 15%, 17%, 18%, 19.5%, 21.2%, 25%, 27.5% or 30%, preferably 5-20%.

在本發明中,所述油基濃縮液中c組分的重量百分比為20~90%,例如20%、21%、25%、32%、40%、50%、55%、60%、68%、72%、80%、85%或90%,較佳為30~80%;In the present invention, the weight percentage of the component c in the oil-based concentrated liquid is 20 to 90%, such as 20%, 21%, 25%, 32%, 40%, 50%, 55%, 60%, 68 %, 72%, 80%, 85% or 90%, preferably 30 ~ 80%;

在本發明中,通過使用所述c組分中的酯的任意一種或至少兩種組合,能夠避免傳統植物油的添加。當所述c組分含量範圍在較佳為30~80%時,既能夠完全溶解百利普芬,又能懸浮賜派滅顆粒,更加有效地避免了粒徑增長風險,克服貯存過程中遇到的問題。In the present invention, by using any one or a combination of at least two of the esters in the c component, the addition of traditional vegetable oil can be avoided. When the content of the c component is preferably in the range of 30 to 80%, it can completely dissolve belipurfin and can also suspend and disperse the granules, which effectively avoids the risk of particle size growth and overcomes the problems encountered during storage. To the problem.

在本發明中,所述油基濃縮液中d組分的重量百分比為1~30%,例如1%、2%、5%、7%、8.7%、10.5%、12%、14%、15%、16.4%、17.5%、19%、21%、23.2%、25%、28%或30%,較佳為5~25%。In the present invention, the weight percentage of the d component in the oil-based concentrated liquid is 1 to 30%, for example, 1%, 2%, 5%, 7%, 8.7%, 10.5%, 12%, 14%, 15 %, 16.4%, 17.5%, 19%, 21%, 23.2%, 25%, 28% or 30%, preferably 5-25%.

在本發明中,所述油基濃縮液中e組分的重量百分比為0~40%,例如0%、2%、5%、7%、9.2%、11%、15%、17%、19%、20%、23%、25%、27%、30%、34%、37%或40%,較佳為0~30%。In the present invention, the weight percentage of the e component in the oil-based concentrated liquid is 0 to 40%, for example, 0%, 2%, 5%, 7%, 9.2%, 11%, 15%, 17%, 19 %, 20%, 23%, 25%, 27%, 30%, 34%, 37% or 40%, preferably 0-30%.

較佳地,所述乳化劑為烷基酚與環氧乙烷和/或環氧丙烷的反應物、乙氧基化的壬基酚、蓖麻油乙氧基化物、多烷氧基化的醇的混合物、烷基鈣鹽、烷基苯磺酸鈣鹽、脫水山梨醇衍生物或聚環氧乙烷脫水山梨醇脂肪酸酯中的任意一種或至少兩種的組合。Preferably, the emulsifier is a reactant of alkylphenol with ethylene oxide and / or propylene oxide, ethoxylated nonylphenol, castor oil ethoxylate, polyalkoxylated alcohol Any one or a combination of at least one of a mixture of an alkyl calcium salt, a calcium alkyl benzene sulfonate, a sorbitan derivative, or a polyethylene oxide sorbitan fatty acid ester.

在本發明中,合適的消泡劑包括所有的在農業化學組合物中常用於此目的的物質。較佳地,所述消泡劑為有機矽消泡劑,較佳矽氧烷消泡劑。In the present invention, suitable defoamers include all substances commonly used for this purpose in agrochemical compositions. Preferably, the defoaming agent is an organosilicon defoamer, and a silicone defoamer is preferred.

在本發明中,合適的防腐劑包括所有的在農業化學組合物中常用於此目的的物質。較佳地,所述防腐劑選自Proxel系列和/或Nipacide系列防腐劑。In the present invention, suitable preservatives include all substances commonly used for this purpose in agrochemical compositions. Preferably, the preservative is selected from Proxel series and / or Nipacide series preservatives.

在本發明中,合適的抗氧化劑包括所有的在農業化學組合物中常用於此目的的物質。較佳地,所述抗氧化劑為2,6-二叔丁基-4-甲基苯酚(BHT)。In the present invention, suitable antioxidants include all substances commonly used for this purpose in agrochemical compositions. Preferably, the antioxidant is 2,6-di-tert-butyl-4-methylphenol (BHT).

在本發明中,合適的著色劑所有的在農業化學組合物中常用於此目的的物質。較佳地,所述著色劑為二氧化鈦、珠光粉、氧化鋅、藍顏料或Pigment Red BBN(即耐曬大紅BBN)中的任意一種或至少兩種的組合。In the present invention, suitable colorants are all substances commonly used for this purpose in agrochemical compositions. Preferably, the colorant is any one or a combination of at least two of titanium dioxide, pearlescent powder, zinc oxide, blue pigment, or Pigment Red BBN (ie, light-fast red BBN).

在本發明中,合適的惰性材料包括所有的在農業化學組合物中常用於此目的、但不起增稠劑作用的物質。較佳地,所述惰性填充材料為尿素、矽酸鹽、硫酸鹽或氧化物中的任意一種或至少兩種的組合。In the present invention, suitable inert materials include all substances commonly used for this purpose in agrochemical compositions but which do not function as thickeners. Preferably, the inert filler material is any one or a combination of at least two of urea, silicate, sulfate or oxide.

較佳地,所述氧化物為金屬氧化物和/或非金屬氧化物。Preferably, the oxide is a metal oxide and / or a non-metal oxide.

另一方面,本發明還提供一種所述的油基濃縮液的製備方法,所述製備方法為:將所述a組分、b組分、c組分、d組分和任選的e組分攪拌混合,研磨得到所述油基濃縮液。In another aspect, the present invention also provides a method for preparing the oil-based concentrated solution, the method for preparing is: combining the component a, component b, component c, component d, and optional component e Mix with stirring and grind to obtain the oil-based concentrated solution.

在本發明中,所述油基濃縮液是將b組分經過攪拌完全溶解於c組分中,而後將a組分、d組分和e組分以任意順序加入到上述混合液中得到懸浮體,再經充分研磨得到油基濃縮液。In the present invention, the oil-based concentrated solution is obtained by dissolving the b component in the c component completely by stirring, and then adding the a component, the d component, and the e component to the above-mentioned mixed liquid in any order to obtain suspension. And then thoroughly ground to obtain an oil-based concentrated solution.

較佳地,所述研磨在10-50℃下進行,例如10℃、15℃、20℃、25℃、30℃、35℃、40℃、45℃或50℃,較佳為15-45℃。Preferably, the grinding is performed at 10-50 ° C, such as 10 ° C, 15 ° C, 20 ° C, 25 ° C, 30 ° C, 35 ° C, 40 ° C, 45 ° C or 50 ° C, preferably 15-45 ° C. .

較佳地,所述研磨為研磨至所述油基濃縮液的固體顆粒粒徑D90≤10 μm,例如0.4 μm、0.8 μm、1 μm、2 μm、3 μm、4 μm、5 μm、6 μm、7 μm、8 μm、9 μm或10 μm,較佳為D90≤5 μm。Preferably, the grinding is grinding to a solid particle size D90≤10 μm of the oil-based concentrated liquid, for example, 0.4 μm, 0.8 μm, 1 μm, 2 μm, 3 μm, 4 μm, 5 μm, 6 μm , 7 μm, 8 μm, 9 μm, or 10 μm, preferably D90 ≦ 5 μm.

在本發明中,所述油基濃縮液固體顆粒平均尺寸小於10 μm,在常溫貯存和/或熱貯條件下,顆粒粒徑變化很小,增長相對緩慢,較長時間內保持穩定。In the present invention, the average size of the solid particles of the oil-based concentrated liquid is less than 10 μm. Under normal temperature storage and / or hot storage conditions, the particle size changes little, grows relatively slowly, and remains stable for a long time.

在本發明中,所述製備方法與現有的微膠囊懸浮劑或者微膠囊懸浮劑-懸浮劑的製備方法相比配方成本低,工藝簡單,對設備要求低,加工效率高。In the present invention, the preparation method has lower formulation cost, simple process, lower equipment requirements, and higher processing efficiency than existing microcapsule suspension agents or microcapsule suspension agent-suspension agent preparation methods.

另一方面,本發明提供一種噴霧液,所述噴霧液包括如上所述的油基濃縮液。In another aspect, the present invention provides a spray liquid comprising the oil-based concentrated liquid as described above.

本發明中,通過用水稀釋,可將本發明油基濃縮液轉化為均一的噴霧液。所述噴霧液通過常規的方法施用,例如通過噴霧、注射、點滴或傾倒進行施用。In the present invention, the oil-based concentrated liquid of the present invention can be converted into a uniform spray liquid by dilution with water. The spray is applied by conventional methods, for example by spraying, injection, drip or pouring.

在本發明中,當用水稀釋所述油基濃縮液時,既沒有明顯的乳狀液分層,也沒有破壞性的絮凝作用,也沒有百利普芬的析晶現象,具有非常良好的理化性質。In the present invention, when the oil-based concentrated solution is diluted with water, there is no obvious emulsion layering, no destructive flocculation, and no crystallization phenomenon of belipfine, and it has very good physical and chemical properties. nature.

另一方面,本發明提供一種如上所述的油基濃縮液施用於植物和/或其生長環境的用途。In another aspect, the present invention provides the use of an oil-based concentrated solution as described above for applying to a plant and / or its growing environment.

本發明的油基濃縮液施用於植物時,能夠被植物吸收,增強植物施用部位對於油基濃縮液的滲透,提高施用效率,增強賜派滅與百利普芬複配活性物的生物利用度,降低其利用量。When the oil-based concentrated solution of the present invention is applied to a plant, the oil-based concentrated solution can be absorbed by the plant, enhance the penetration of the oil-based concentrated solution by the plant application site, improve the application efficiency, and enhance the bioavailability of Ciprofen and Paliprofen compound , Reduce its utilization.

另一方面,本發明提供一種如上所述的油基濃縮液用於防治昆蟲的用途。In another aspect, the present invention provides the use of the oil-based concentrated liquid as described above for controlling insects.

本發明的油基濃縮液穩定性高,能夠提高其主要活性成分中賜派滅與百利普芬複配的活性,提升對於昆蟲的防治效果。The oil-based concentrated liquid of the present invention has high stability, can increase the activity of Ciparam and belipofen in its main active ingredients, and enhances the effect of controlling insects.

較佳地,所述防治的昆蟲為鱗翅目害蟲、雙翅目害蟲、半翅目害蟲或同翅目害蟲中的任意一種或至少兩種。Preferably, the insects to be controlled are any one or at least two of Lepidoptera pests, Diptera pests, Hemiptera pests or Homoptera pests.

鱗翅目害蟲,如埃及鑽夜蛾(Earias insulana)、菜粉蝶(Pieris rapae Linnaeus)、蒼螟(Herpetogramma licarsisalis Walker)、草地貪夜蛾(Spodoptera fugiperda)、草地粘蟲(Spodoptera frugiperda)、尺蠖(Rachiplusia nu)、大豆夜蛾(Pseudoplusia includens)、稻蛀莖夜蛾(Sesamia inferens)、稻縱卷葉螟(Cnaphalocrocis medinalis Guenee)、豆茄野螟(Maruca testulalis)、二化螟(Cirphisunipuncta)、番茄斑潛蠅(Tuta absoluta)、粉斑夜蛾(Trichoplusia ni)、粉莖螟(Sesamianonagrioides)、粉紋夜蛾(Trichoplusia ni)、梨豆夜蛾(Anticarsia gemmatalis)、梨小食心蟲(Grapholitha molesta)、馬鈴薯塊莖蛾(Phthorimaea operculella)、麥蛾(Sitotroga cerealella)、棉斑實蛾(Earias vittella Fabricius)、棉褐帶卷蛾(Adoxophyes orana)、棉紅鈴蟲(Pectinophoragossypiella Saunders)、棉鈴蟲(Heliothis armigera)、棉葉波紋夜蛾(Alabama argi llacea)、模毒蛾(Lymantria monacha)、蘋果小卷蛾(Cydia pomonella)、蘋褐卷蛾(Pandemis heparana)、葡萄小卷葉蛾(Lobesia botrana)、葡萄長須卷蛾(Sparganothis pilleriana)、葡萄小食心蟲(Endopiza vriteana Clemens)、三化螟(Scirpophaga incertulas)、甜菜夜蛾(Spodopteraexigua Hübner)、斜紋夜蛾(Spodopteraritura)、煙草粉斑螟(Ephestia elutella)、煙芽夜蛾(Heliothis virescens)、夜小卷蛾(Epinotia aporema)、衣蛾(Tineola bisselliella)、印度穀斑蝶(Plodiainterpunctella)、玉米螟(Ostrinianubilalis Hübner)。Lepidopteran pests, such as Earias insulana, Pieris rapae Linnaeus, Herpetogramma licarsisalis Walker, Spodoptera fugiperda, Spodoptera frugiperda, and Rachiplusia nu), Pseudoplusia includens, Sesamia inferens, Cnaphalocrocis medinalis Guenee, Maruca testulalis, Cirphisunipuncta, Tomato spot Tuta absoluta, Trichoplusia ni, Sesamianonagrioides, Trichoplusia ni, Anticarsia gemmatalis, Grapholitha molesta, potato Tuber moth (Phthorimaea operculella), wheat moth (Sitotroga cerealella), cotton spot moth (Earias vittella Fabricius), cotton brown band moth (Adoxophyes orana), cotton bollworm (Pectinophoragossypiella Saunders), cotton bollworm (Heliothis armigera), Alabama argi llacea, Lymantria monacha, Cydia pomonella, Pandemis heparana), Lobesia botrana, Sparganothis pilleriana, Endopiza vriteana Clemens, Scirpophaga incertulas, Spodopteraexigua Hübner, Spodoptera exigua (Spodopteraritura), Tobacco mealworm (Ephestia elutella), Tobacco bud moth (Heliothis virescens), Eupnotia aporema, Tineola bisselliella, Plodiainterpunctella, Ostrinianubilalis Hübner).

雙翅目害蟲,如埃及伊蚊(Aedes aegypti)、菜潛蠅(Liriomyza brassicae)、赤尾麻蠅(Sarcophaga haemorrhoidalis)、刺舌蠅(Glossina morsi tans)、蔥蠅(Phorbia antiqua)、地中海實蠅(Ceratitis capitata)、甘藍地種蠅(Delia radicum)、瓜蠅(Dacuscucurbi tae)、馬蠅(Tabanus lineola)、紅頭麗蠅(Calliphora vricina)、胡蘿蔔莖蠅(Psila rosae)、桔小實蠅(Bactrocera dorsalis)、狂怒庫蠓(Culicoides furens)、剌擾伊蚊(Aedes vexans)、藍橘繞實蠅(Rhagoletis mendax)、麗蠅(Chrysomya spp.)、鹿蠅(Chrysops discalis)、蘿卡蠅(Phorbia brassicae)、麥紅吸漿蟲(Si todiplosis mosellana)、美國潛葉蠅(Liriomyza trifolii)、蘋果實蠅(Rhagoletis pomonella)、潛蠅屬(Hippelates)、桃實蠅(Bactrocera zonata)、天仙子泉蠅(Pegomya hysocyami)、甜菜泉蠅(Pegomya betae)、銅綠蠅(Lucilia cuprina)、致倦庫蚊(Culexquinquefasciatus)。Diptera pests such as Aedes aegypti, Liriomyza brassicae, Sarcophaga haemorrhoidalis, Glossina morsi tans, Phorbia antiqua, Ceratitis capitata), cabbage fly (Delia radicum), melon fly (Dacuscucurbi tae), horsefly (Tabanus lineola), calliphora vricina, carrot stem fly (Psila rosae), orange fruit fly (Bactrocera dorsalis) , Culicoides furens, Aedes vexans, Rhagoletis mendax, Chrysomya spp., Chrysops discalis, Phorbia brassicae , Si todiplosis mosellana, Liriomyza trifolii, Rhagoletis pomonella, Hippelates, Bactrocera zonata, Pegomya hysocyami , Beet fly (Pegomya betae), Lucilia cuprina, Culexquinquefasciatus.

半翅目和同翅目害蟲,如白背飛虱(Sogatellafurcifera Horvrath)、白粉虱(Trialeurodes vaporariorum)、吹綿蚧(Ieryapurchasi Maskell)、吹棉蚧(Iceryapurchasi)、大豆蚜(Aphis glycines)、稻飛蝨(Nilapar飛rata lugens)、稻褐飛虱(Nilaparvratalugens)、甘藍蚜(Brevicoryne brassicae)、甘薯粉虱(Bemisia tabaci)、柑桔木虱(Diaphorina citri)、黑尾葉蟬(Nephotettix nigropictus)、紅蠟蚧(Ceroplastesrubens)、紅圓蚧(Aonidiella aurantii)、灰飛虱(Laodelphax striatellus)、豇豆蚜(Aphis craccivrora Koch)、麥長管蚜(Macrosiphum avenae)、蘋果蚜(Aphis pomi)、蘋木虱(Psylla mali)、桃短尾蚜(Brachycaudus persicae)、桃蚜(Myzuspersicae Sulzer)、豌豆蚜(Acyrthisiphon pisum Harris)、溫室白粉虱(Trialeurodes vaporariorum)、煙粉虱(Bemisia tabaci Gennadius)、葉蟬(Empoasca spp.)、玉米花翅飛虱(Peregrinus maidis)、玉米蠟蟬(Peregrinus maidisAshmead)、玉米蚜(Rhopalosiphum maidis)、縱條稻飛蝨(Sogatodes orizicola Muir)。Hemiptera and Homoptera pests such as Sogatellafurcifera Horvrath, Trialeurodes vaporariorum, Ieryapurchasi Maskell, Iceryapurchasi, Aphis glycines, Rice fly Lice (Nilapar fly rata lugens), rice brown fly (Nilaparvratalugens), cabbage aphid (Brevicoryne brassicae), sweet potato whitefly (Bemisia tabaci), citrus psyllid (Diaphorina citri), black-tailed leafhopper (Nephotettix nigropictus), red Ceroplastesrubens, Aonidiella aurantii, Laodelphax striatellus, Aphis craccivrora Koch, Macrosiphum avenae, Apple aphid (Aphis pomi), Apple psyllid (Aphis pomi) Psylla mali), Brachycaudus persicae, Myzuspersicae Sulzer, Acyrthisiphon pisum Harris, Trialeurodes vaporariorum, Bemisia tabaci Gennadius, Leafhopper (Empoasca spp) .), Peregrinus maidis, Peregrinus maidisAshmead, Rhopalosiphum maidis, Sogatodes orizico la Muir).

本發明的油基濃縮液特別適用於防治煙粉虱、飛虱、蚜蟲、介殼蟲、薊馬、稻縱卷葉螟、三化螟、紅蜘蛛、斜紋夜蛾、菜青蟲、小菜蛾、甜菜夜蛾、黃條跳甲或茶小綠葉蟬。進一步特別適合用於防治煙粉虱和/或飛虱。The oil-based concentrated solution of the present invention is particularly suitable for controlling Bemisia tabaci, planthoppers, aphids, scale insects, thrips, rice leaf rollers, cockroaches, red spiders, Spodoptera litura, cabbage worm, diamondback moth, beet Spodoptera litura, yellow-striped beetle, or tea leafhopper. It is further particularly suitable for controlling whitefly and / or planthopper.

相對於現有技術,本發明具有以下有益效果: (1) 本發明的油基濃縮液,與其他現有劑型相比,能有效的控制賜派滅在儲存過程中粒徑增長解決了賜派滅懸浮顆粒粒徑增長的問題,同時百利普芬能以分子狀態穩定的存在於濃縮液中,不會有晶體析出,兩者活性物之間不相互影響,保持各自的狀態於濃縮物中,更大程度的保持與發揮了兩者的生物活性。 (2) 本發明的油基濃縮液,克服常規條件的束縛,不含有增稠劑植物油或礦物油,具有非常良好的穩定性,尤其適合用於提高賜派滅活性物與百利普芬複配製劑的穩定性。 (3) 本發明的油基濃縮液,具有良好的理化性質。當用水稀釋本發明的濃縮液時,既沒有明顯的乳狀液分層,也沒有破壞性的絮凝作用,而且避免了百利普芬的析晶現象。 (4) 本發明的油基濃縮液,提升了賜派滅與百利普芬的生物活性,減少二者的使用量,增強生物利用度,最終降低成本,並且對煙粉虱具有良好的防治效果,高濃度給藥25天後對煙粉虱成蟲的防治效果可達到95%以上,對煙粉虱若蟲的防治效果可達85%以上。 (5) 本發明的油基濃縮液製備方法工藝簡單,對設備要求低,加工效率高,利於進行工業化規模生產,大大降低了生產成本。Compared with the prior art, the present invention has the following beneficial effects: (1) Compared with other existing dosage forms, the oil-based concentrated liquid of the present invention can effectively control the particle size increase during storage and solve the problem of suspension The problem of particle size increase, at the same time, Paliprofen can exist in the concentrated solution in a stable molecular state without crystal precipitation, and the two active substances do not affect each other, maintaining their respective states in the concentrate. The biological activity of both is maintained and exerted to a large extent. (2) The oil-based concentrated liquid of the present invention overcomes the constraints of conventional conditions, does not contain thickener vegetable oil or mineral oil, and has very good stability, and is particularly suitable for improving the active ingredients of Papex and Paliprofen. Formulation stability. (3) The oil-based concentrated liquid of the present invention has good physical and chemical properties. When the concentrated solution of the present invention is diluted with water, there is neither obvious emulsion delamination nor destructive flocculation, and the crystallization phenomenon of paliprofen is avoided. (4) The oil-based concentrated liquid of the present invention improves the bioactivity of Cipamir and Peripipen, reduces the use of both, enhances bioavailability, ultimately reduces costs, and has good control of Bemisia tabaci Effect, 25 days after high-concentration administration, the control effect on Bemisia tabaci adults can reach more than 95%, and the control effect on Bemisia tabaci nymphs can reach more than 85%. (5) The method for preparing the oil-based concentrated liquid of the present invention is simple in process, low in equipment requirements, high in processing efficiency, favorable for industrial-scale production, and greatly reduced production costs.

下面通過具體實施方式來進一步說明本發明的技術方案。本領域技術人員應該明瞭,所述實施例僅僅是幫助理解本發明,不應視為對本發明的具體限制。The technical solutions of the present invention will be further described below through specific embodiments. Those skilled in the art should understand that the embodiments are merely to help understand the present invention and should not be regarded as a specific limitation to the present invention.

以下實施例中所用物質本領域技術人員均可通過常規管道獲得。The substances used in the following examples can be obtained by those skilled in the art through conventional pipelines.

實施例1 在本實施例中,油基濃縮液包括如下組分: Embodiment 1 In this embodiment, the oil-based concentrated liquid includes the following components:

製備方法如下:將百利普芬加入到油酸乙酯中,充分攪拌使百利普芬完全溶解在油酸乙酯中。其他物料任意順序加入到上述混合液中,攪拌均勻得到懸浮液。在45℃以下經砂磨機一級粗磨,二級細磨,得到懸浮顆粒D90小於5 μm的油基濃縮液。The preparation method is as follows: adding belipurfin to ethyl oleate, and thoroughly stirring to completely dissolve belipurfin in ethyl oleate. Other materials are added to the above mixture in any order, and stirred to obtain a suspension. An oil-based concentrated solution with suspended particles D90 of less than 5 μm was obtained by rough grinding and fine grinding by a sand mill below 45 ° C.

對比例1 在本對比例中,油基濃縮液包括如下組分: 賜派滅 10% 百利普芬 10% 聚氧乙烯-山梨醇油酸酯 15% 多烷氧基化的醇的混合物 7% 木質素磺酸鹽 3% 聚二甲基矽氧烷 1% 2,6-二叔丁基-4-甲基苯酚 0.5% 植物油(大豆油) 53.5%Comparative Example 1 In this comparative example, the oil-based concentrated solution includes the following components: 10% Papex 10% Polyoxyethylene-sorbitan 15% Polyalkoxylated alcohol mixture 7 % Lignin sulfonate 3% Polydimethylsiloxane 1% 2,6-Di-tert-butyl-4-methylphenol 0.5% Vegetable oil (soy oil) 53.5%

製備方法如下:將原物料任意順序加入到大豆油中,攪拌均勻得到懸浮液。在45℃以下經砂磨機一級粗磨,二級細磨,得到懸浮顆粒D90小於5 μm的油懸浮劑。The preparation method is as follows: the raw materials are added to the soybean oil in any order, and stirred to obtain a suspension. An oil suspension agent with a suspended particle D90 of less than 5 μm was obtained by rough grinding and fine grinding by a sand mill below 45 ° C.

按以上相同配置方法製備實施例2-7和對比例2-7,其成分以及用量如表1所示。Examples 2-7 and Comparative Examples 2-7 were prepared according to the same configuration method as above, and the components and amounts are shown in Table 1.

表1 Table 1

對比例8 Comparative Example 8

製備方法如下:將除了黃原膠和生物殺菌劑以外的其他物料任意順序加入到水中,攪拌均勻得到懸浮液。在45℃以下經砂磨機一級粗磨,二級細磨,得到懸浮顆粒D90小於5 μm的水基濃縮液。再按比例加入黃原膠和生物殺菌劑,攪拌直至均勻,即得水懸浮劑。The preparation method is as follows: materials other than xanthan gum and a biocide are added to the water in any order and stirred to obtain a suspension. The coarse-grinding and fine-grinding of the sand mill were carried out below 45 ° C to obtain a water-based concentrated solution with suspended particles D90 of less than 5 μm. Then add the xanthan gum and the biocide in proportion, and stir until uniform to obtain an aqueous suspension.

將上述實施例1-7製備的樣品和對比例1-8樣品長期貯存,進行測試比較樣品流動性和粒徑增長比較。測試方法為:將上述7個樣品放置在54℃烘箱中放置14天、28天後觀察樣品流動性和用瑪爾文粒徑儀測試貯存前後粒徑大小。具體流動性測量結果如表2,粒徑測量結果如表3:The samples prepared in the above Examples 1-7 and the comparative examples 1-8 were stored for a long time, and tests were performed to compare the fluidity and particle size growth of the samples. The test method is: put the above 7 samples in a 54 ° C oven for 14 days and 28 days to observe the sample fluidity and test the particle size before and after storage with a Marvin particle size analyzer. The specific fluidity measurement results are shown in Table 2 and the particle size measurement results are shown in Table 3:

表 2 Table 2

表2的實驗表明常規的水懸浮劑和油懸浮劑,由於百利普芬熔點較低,在54℃熱貯條件下發生熔化,熔化的原藥油滴相互聚合而導致樣品理化性能發生變化。而本發明的油基濃縮液賜派滅與百利普芬複配製劑解決了這一問題。The experiments in Table 2 show that the conventional water suspension and oil suspension agents, due to the lower melting point of belipfine, melted under the condition of hot storage at 54 ° C, and the molten crude drug oil droplets polymerized with each other, resulting in changes in the physical and chemical properties of the samples. The oil-based concentrated solution of the present invention, Ciprofen and Periperfin, solves this problem.

表 3 table 3

表3的實驗資料表明,本發明的賜派滅與百利普芬複配的油基濃縮液有效地控制了懸浮顆粒高溫長期貯存的粒徑增長速度,提高了油基濃縮液的穩定性。The experimental data in Table 3 show that the oil-based concentrated solution of Cipaim and Paliprofen of the present invention effectively controls the growth rate of the suspended particles in high temperature and long-term storage, and improves the stability of the oil-based concentrated solution.

應用例1 在該應用例中,對以上實施例1-7以及對比例1-8製備的樣品進行生物活性測試,方法如下:Application Example 1 In this application example, the biological activity test was performed on the samples prepared in the above Examples 1-7 and Comparative Examples 1-8, as follows:

試驗物件:番茄煙粉虱Test object: Bemisia tabaci

採用上述實施例1-7、對比例1-8的樣品進行試驗,在番茄種植區域採用噴霧法,在低齡蟲高峰期施藥,正反面均勻噴霧,每個處理重複3次。The above-mentioned examples 1-7 and comparative examples 1-8 were used for testing. The spray method was used in the tomato planting area. The pesticide was applied at the peak of the young instar, and the front and back were sprayed uniformly. Each treatment was repeated 3 times.

成蟲調查採用每個區域標定8株番茄,每株標定2個大枝,在清晨成蟲不活躍時調查大枝上成蟲數。Adults were surveyed using 8 tomato plants per area and 2 large branches per plant. The number of adults on the large branches was investigated when the adults were not active in the early morning.

若蟲調查採用在未標定的5株番茄的上中下各採集3片葉子,共15片,分別記錄這15片葉子上的若蟲數。For the nymph survey, three leaves were collected from the top, middle, and bottom of five uncalibrated tomato plants for a total of 15 leaves, and the number of nymphs on these 15 leaves was recorded.

調查給藥後7、14、25天以後植株上的成蟲數和若蟲數。The number of adults and nymphs on the plants was investigated after 7, 14, and 25 days after the administration.

藥效計算方法: 蟲口減退率=×100% 防治效果=×100%Effectiveness calculation method: Decline rate of insects = × 100% control effect = × 100%

對煙粉虱成蟲防效(防治效果)結果如表4所示:The results of the control effect (control effect) on Bemisia tabaci adults are shown in Table 4:

表 4 Table 4

本發明的賜派滅與百利普芬複配的油基濃縮液對煙粉虱成蟲有優異的防治效果,高劑量給藥25天後對煙粉虱成蟲的防治效果可達到95%以上。The oil-based concentrated liquid compounded by Cipaifen and Bailipufen of the present invention has excellent control effect on Bemisia tabaci adults. After 25 days of high dose administration, the control effect on Bemisia tabaci adults can reach more than 95%.

對煙粉虱若蟲的防治效果如表5所示:The control effect on Bemisia tabaci nymphs is shown in Table 5:

表5 table 5

本發明的賜派滅與百利普芬複配的油基濃縮液對煙粉虱若蟲有優異的防治效果,高劑量給藥25天後其對煙粉虱若蟲的防治效果可達85%以上。The oil-based concentrated solution of Cipaimex and belipipen of the present invention has excellent control effect on Bemisia tabaci nymphs. After 25 days of high-dose administration, the control effect on Bemisia tabaci nymphs can reach more than 85%. .

申請人聲明,本發明通過上述實施例來說明本發明的油基濃縮液及其製備方法和用途,但本發明並不局限於上述實施例,即不意味著本發明必須依賴上述實施例才能實施。所屬技術領域的技術人員應該明瞭,對本發明的任何改進,對本發明產品各原料的等效替換及輔助成分的添加、具體方式的選擇等,均落在本發明的保護範圍和公開範圍之內。The applicant states that the present invention illustrates the oil-based concentrated solution of the present invention, its preparation method, and application through the above examples, but the present invention is not limited to the above examples, that is, it does not mean that the present invention must rely on the above examples to be implemented . Those skilled in the art should know that any improvement to the present invention, equivalent replacement of the raw materials of the products of the present invention, addition of auxiliary components, selection of specific methods, etc., all fall within the scope of protection and disclosure of the present invention.

no

no

Claims (10)

一種油基濃縮液,其特徵在於,所述油基濃縮液包括如下組分: a 組分:至少一種室溫下為固體的賜派滅(spirotetramat)活性物; b 組分:至少一種室溫下為固體的百利普芬(pyriproxyfen)活性物; c 組分:至少一種具有通式R1-COO-R2和/或R1-COO-R2-OOC-R1脂肪酸酯,其中R1為具有10~25個碳原子的烷基和/或烯基,R2為具有1~10個碳原子的烷基; d 組分:至少一種非離子表面活性劑和/或至少一種陰離子表面活性劑; 任選地 e 組分:一種或至少兩種選自乳化劑、消泡劑、防腐劑、抗氧化劑、著色劑或惰性填充材料的添加劑; 其中百利普芬是以分子狀態溶解於c組分中,賜派滅是以顆粒狀態懸浮於c組分中。An oil-based concentrated liquid, characterized in that the oil-based concentrated liquid includes the following components: a component: at least one spirotetramat active substance which is solid at room temperature; b component: at least one room temperature The following is a solid pyriproxyfen active; c Component: at least one fatty acid ester having the general formula R1-COO-R2 and / or R1-COO-R2-OOC-R1, where R1 is An alkyl and / or alkenyl group of 25 carbon atoms, R2 is an alkyl group having 1 to 10 carbon atoms; d component: at least one non-ionic surfactant and / or at least one anionic surfactant; optionally e component: one or at least two additives selected from emulsifiers, defoamers, preservatives, antioxidants, colorants, or inert filler materials; where belipfen is dissolved in the c component in a molecular state, and Pixi is suspended in the c component in the form of particles. 根據請求項1所述的油基濃縮液,其特徵在於,所述油基濃縮液包括 如下重量百分比的組分:0.1~30%的所述a組分、0.1~30%的所述b組分、20~90%的所述c組分、1~30%的所述d組分和0~40%的所述e組分;The oil-based concentrated liquid according to claim 1, wherein the oil-based concentrated liquid includes the following components in weight percentages: 0.1 to 30% of the component a, and 0.1 to 30% of the component b. 20% to 90% of the c component, 1 to 30% of the d component and 0 to 40% of the e component; 根據請求項1或2所述的油基濃縮液,其特徵在於,所述c組分中R1為具有12~20個碳原子的烷基和/或烯基,較佳具有12~18個碳原子的烷基和/或烯基;R2為具有2~8個碳原子的烷基,較佳具有2~6個碳原子的烷基; 較佳地,所述烷基為直鏈烷基或支鏈烷基。The oil-based concentrate according to claim 1 or 2, characterized in that R1 in the c component is an alkyl group and / or an alkenyl group having 12 to 20 carbon atoms, preferably 12 to 18 carbon atoms Atomic alkyl and / or alkenyl; R2 is an alkyl having 2 to 8 carbon atoms, preferably an alkyl having 2 to 6 carbon atoms; preferably, the alkyl is a straight-chain alkyl or Branched alkyl. 根據請求項1-3中任一項所述的油基濃縮液,其特徵在於,所述c組分為油酸乙酯、油酸丁酯、月桂酸己酯、棕櫚酸乙二酯或亞油酸戊二酯中的任意一種或至少兩種的組合。The oil-based concentrated liquid according to any one of claims 1-3, wherein the component c is ethyl oleate, butyl oleate, hexyl laurate, ethylene palmitate, or propylene Any one or a combination of at least two of glutaryl oleate. 根據請求項1-4中任一項所述的油基濃縮液,其特徵在於,所述非離子表面活性劑選自甲基丙烯酸與甲基丙烯酸酯的共聚物、脂肪醇與環氧乙烷和/或環氧丙烷的聚合物、環氧乙烷-環氧丙烷嵌段共聚物、脂肪醇聚氧乙烯醚、聚乙烯醇、烷基糖苷、聚乙烯吡咯烷酮、烷基乙氧基化物、烷基芳基乙氧基化物或吐溫中的任意一種或至少兩種的組合; 較佳地,所述陰離子表面活性劑選自木質素磺酸鹽、琥珀酸磺酸鹽、萘磺酸鹽甲醛縮聚物、三苯乙烯乙氧基化物的硫酸鹽、三苯乙烯乙氧基化物的磷酸鹽或聚羧酸鹽中的任意一種或至少兩種的組合。The oil-based concentrate according to any one of claims 1-4, wherein the non-ionic surfactant is selected from the group consisting of a copolymer of methacrylic acid and methacrylate, a fatty alcohol and ethylene oxide. And / or propylene oxide polymers, ethylene oxide-propylene oxide block copolymers, fatty alcohol polyoxyethylene ethers, polyvinyl alcohol, alkyl glycosides, polyvinyl pyrrolidone, alkyl ethoxylates, alkane Any one or a combination of at least two of an aryl ethoxylate or Tween; preferably, the anionic surfactant is selected from lignin sulfonate, succinate sulfonate, naphthalene sulfonate formaldehyde Any one or a combination of at least two of a polycondensate, a sulfate of tristyrene ethoxylate, a phosphate of tristyrene ethoxylate, or a polycarboxylate. 根據請求項1-5中任一項所述的油基濃縮液,其特徵在於,所述油基濃縮液中a組分的重量百分比為5~20%; 較佳地,所述油基濃縮液中b組分的重量百分比為5~20%; 較佳地,所述油基濃縮液中c組分的重量百分比為30~80%; 較佳地,所述油基濃縮液中d組分的重量百分比為2~20%; 較佳地,所述油基濃縮液中e組分的重量百分比為0~30%。The oil-based concentrated liquid according to any one of claims 1-5, characterized in that the weight percentage of component a in the oil-based concentrated liquid is 5 to 20%; preferably, the oil-based concentrated The weight percentage of component b in the liquid is 5 to 20%; preferably, the weight percentage of component c in the oil-based concentrated solution is 30 to 80%; preferably, the group d in the oil-based concentrated solution is The weight percentage of the cent is 2 to 20%; preferably, the weight percentage of the e component in the oil-based concentrated solution is 0 to 30%. 根據請求項1-6中任一項所述的油基濃縮液的製備方法,其特徵在於,所述製備方法為:將所述a組分、b組分、c組分、d組分和任選的e組分攪拌混合,研磨得到所述油基濃縮液; 較佳地,所述研磨在10-50℃下進行,較佳為15-45℃; 較佳地,所述研磨為研磨至所述油基濃縮液的固體顆粒粒徑D90≤10 μm,較佳為D90≤5 μm。The method for preparing an oil-based concentrated liquid according to any one of claims 1-6, wherein the method for preparing is: combining the a component, the b component, the c component, the d component, and Optional component e is stirred and mixed to obtain the oil-based concentrated liquid; preferably, the grinding is performed at 10-50 ° C, preferably 15-45 ° C; preferably, the grinding is grinding The particle diameter of the solid particles of the oil-based concentrated liquid is D90 ≦ 10 μm, preferably D90 ≦ 5 μm. 一種噴霧液,其特徵在於,所述噴霧液包括如請求項1-6中任一項所述的油基濃縮液。A spray liquid, characterized in that the spray liquid comprises the oil-based concentrated liquid according to any one of claims 1-6. 一種根據請求項1-6中任一項所述的油基濃縮液施用於植物和/或其生長環境的用途。A use of the oil-based concentrated liquid according to any one of claims 1-6 to a plant and / or a growth environment thereof. 一種根據請求項1-6中任一項所述的油基濃縮液用於防治昆蟲的用途; 較佳地,所述防治的昆蟲為鱗翅目害蟲、雙翅目害蟲、半翅目害蟲或同翅目害蟲中的任意一種或至少兩種; 較佳地,所述防治的昆蟲為煙粉虱和/或飛虱。A use of the oil-based concentrated liquid according to any one of claims 1 to 6 for controlling insects; preferably, the insects to be controlled are Lepidoptera pests, Diptera pests, Hemiptera pests or the same Any one or at least two of the winged pests; Preferably, the insects to be controlled are whitefly and / or planthopper.
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