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CN1229020C - Nicotine microcapsule suspoemulsion and preparation method thereof - Google Patents

Nicotine microcapsule suspoemulsion and preparation method thereof Download PDF

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CN1229020C
CN1229020C CN 03139131 CN03139131A CN1229020C CN 1229020 C CN1229020 C CN 1229020C CN 03139131 CN03139131 CN 03139131 CN 03139131 A CN03139131 A CN 03139131A CN 1229020 C CN1229020 C CN 1229020C
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glue
nicotine
vegetable
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suspoemulsion
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CN1513311A (en
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张天良
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Zhong Weide
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Abstract

The invention relates to a nicotine microcapsule suspoemulsion and its preparation method, the nicotine microcapsule suspoemulsion is to regard nicotine as the active ingredient, and contain surfactant active, vegetable oil, auxiliary agent, solvent, water, also contain the composition of two kinds or more than two kinds of hydrolysates in animal glue, vegetable glue and marine product glue at the same time, its preparation method is to add auxiliary agent, vegetable oil, surfactant into the oily liquid nicotine, add solvent to dilute, heat to 50-80 duC, stir constantly at the same time, add a certain amount of water; respectively hydrolyzing two or more kinds of glue in the animal glue, the vegetable glue and the marine product glue, respectively heating to 50-80 ℃, filtering, mixing, uniformly stirring, adding into the preparation solution, mixing and stirring at the rotating speed of 200 plus materials and 600 rpm, and naturally cooling for 2 hours; it has slow decomposition under visible light and long drug action time, and can be widely used on pollution-free green economic crops.

Description

烟碱微胶囊悬乳剂及其制备方法Nicotine microcapsule suspoemulsion and preparation method thereof

(一)技术领域:(1) Technical field:

本发明涉及农药的剂型技术领域,具体地讲是一种烟碱微胶囊悬乳剂及其制备方法。The invention relates to the technical field of pesticide formulations, in particular to a nicotine microcapsule suspoemulsion and a preparation method thereof.

(二)背景技术:(two) background technology:

众所周知,烟碱是从烟草中直接提出的,具有高效、低毒、无残留的特点,适合无公害绿色食品施用,但烟碱本身见光分解,在阳光下半小时内挥发完。As we all know, nicotine is extracted directly from tobacco. It has the characteristics of high efficiency, low toxicity, and no residue. It is suitable for the application of pollution-free green food. However, nicotine itself is decomposed by light and volatilizes within half an hour in the sun.

(三)发明内容:(3) Contents of the invention:

本发明的目的旨在克服上述已有技术的不足,而提供一种烟碱微胶囊悬乳剂。The purpose of the present invention is to overcome the shortcomings of the above-mentioned prior art, and provide a nicotine microcapsule suspoemulsion.

本发明的另一目的是提供烟碱微胶囊悬乳剂的制备方法。Another object of the present invention is to provide a preparation method of nicotine microcapsule suspoemulsion.

本发明主要解决了烟碱见光分解快的问题。The invention mainly solves the problem of fast decomposition of nicotine upon exposure to light.

本发明的烟碱微胶囊悬乳剂由于其囊皮完全由天然的高分子聚合物组成,可以在空气中完全裂解,对植物本身和环境无污染,可在蔬菜、瓜果等经济作物上大面积使用。The nicotine microcapsule suspoemulsion of the present invention can be completely cracked in the air because its capsule skin is completely composed of natural high molecular polymers, has no pollution to the plant itself and the environment, and can be used on a large area of economic crops such as vegetables, melons and fruits. use.

为了达到上述目的,本发明是这样实现的:烟碱微胶囊悬乳剂,其特征在于它是以烟碱为有效成份,并含有表面活性剂、植物油、助剂、溶剂、水,同时还含有海产品胶与动物胶和植物胶中的一种或两种的水解物的组合物;表面活性剂为三苯乙基酚聚氧乙烯醚、二苄基联苯酚聚氧乙烯醚,植物油为棉籽油、菜籽油、蓖麻油酸,助剂为十二烷基苯磺酸钙、苯乙基酚聚氧乙烯聚氧丙烯醚、蓖麻油环氧乙烷加成物,溶剂为二甲苯,动物胶为明胶,植物胶为淀粉胶,海产品胶为鱼胶、褐藻酸钠。In order to achieve the above object, the present invention is achieved as follows: nicotine microcapsule suspoemulsion, which is characterized in that it uses nicotine as an active ingredient, and contains surfactants, vegetable oils, additives, solvents, water, and seawater Composition of product gum and hydrolyzate of one or both of animal gum and vegetable gum; surfactant is tristyrylphenol polyoxyethylene ether, dibenzyl biphenol polyoxyethylene ether, and vegetable oil is cottonseed oil , rapeseed oil, ricinoleic acid, additives are calcium dodecylbenzenesulfonate, phenylethylphenol polyoxyethylene polyoxypropylene ether, castor oil ethylene oxide adduct, solvent is xylene, animal glue Gelatin, vegetable glue is starch glue, seafood glue is isinglass and sodium alginate.

本发明的烟碱微胶囊悬乳剂的制备方法,包括如下工艺步骤:The preparation method of the nicotine microcapsule suspoemulsion of the present invention comprises the following process steps:

a,囊核的制作,将油状液烟碱中,加入助剂、植物油、表面活性剂,再加入溶剂进行稀释,加热至60-80℃,同时不断搅拌,再加入一定量的水;助剂为十二烷基苯磺酸钙、苯乙基酚聚氧乙烯聚氧丙烯醚、蓖麻油环氧乙烷加成物,植物油为棉籽油、菜籽油、蓖麻油酸,表面活性剂为三苯乙基酚聚氧乙烯醚、二苄基联苯酚聚氧乙烯醚,溶剂为二甲苯;a, the production of the capsule core, adding additives, vegetable oil, and surfactant to the oily liquid nicotine, then adding a solvent to dilute, heating to 60-80°C, stirring continuously at the same time, and then adding a certain amount of water; additives Calcium dodecylbenzenesulfonate, phenylethylphenol polyoxyethylene polyoxypropylene ether, castor oil ethylene oxide adduct, vegetable oil is cottonseed oil, rapeseed oil, ricinoleic acid, surfactant is three Phenylphenol polyoxyethylene ether, dibenzyl biphenol polyoxyethylene ether, the solvent is xylene;

b,囊皮的制作,将海产品胶与动物胶和植物胶中的一种或两种胶分别先进行各类胶的水解,分别加热至60-80℃,过滤后混合,搅拌均匀即可;海产品胶为鱼胶、褐藻酸钠,动物胶为明胶,植物胶为淀粉胶;b. For the production of capsule skin, hydrolyze seafood glue, one or two kinds of glue from animal glue and vegetable glue, respectively, heat them to 60-80°C, filter and mix, and stir evenly. The seafood glue is isinglass and sodium alginate, the animal glue is gelatin, and the vegetable glue is starch glue;

c,微胶囊制剂,将步骤b的囊皮原料倒入步骤a的囊核的反应釜中,在200-600转/分的转速下混合搅拌,同时自然降温2小时后,进行包装。c, microcapsule preparation, pour the raw material of capsule skin in step b into the reaction kettle of capsule core in step a, mix and stir at a speed of 200-600 rpm, and pack after natural cooling for 2 hours.

本发明的烟碱微胶囊悬乳剂的制备方法,其所述的囊皮采用动物胶和植物胶时,其囊皮孔小且不均匀,达不到按要求规定的释放时间,因此还需加入发泡剂。In the preparation method of the nicotine microcapsule suspoemulsion of the present invention, when animal glue and vegetable glue are used for the capsule skin, the pores of the capsule skin are small and uneven, and the release time specified by the requirements cannot be reached, so it is necessary to add Foaming agent.

本发明的烟碱微胶囊悬乳剂是用有机大分子将农药有效体从外边包起来,得用大分子囊壁的晶格空隙缓慢的释放出来,避免其光解,从而极大的减少原药的用量,延长持效期,可人为地控制其持效期和释放速度;因烟碱见光分解快,因而为控制其药效时间,其微胶囊的粒径较大,一般控制在10-50微米。The nicotine microcapsule suspoemulsion of the present invention uses organic macromolecules to wrap the effective pesticide body from the outside, and releases it slowly through the lattice gap of the macromolecular capsule wall to avoid its photolysis, thereby greatly reducing the cost of the original drug. Dosage, prolonging the effect period, can artificially control its effect period and release speed; because nicotine sees light decomposition quickly, so in order to control its drug effect time, the particle size of its microcapsules is relatively large, generally controlled at 10-50 Micron.

本发明所述的一种烟碱微胶囊悬乳剂及其制备方法与已有技术相比,具有实质性特点和显著进步:1、烟碱微胶囊悬乳剂见光分解慢,从而提高其药效,同时延长药效时间,经试验得知,其原药减少30-50%,防治效果提高10-20%,持效期延长3-10倍;2、烟碱微胶囊悬乳剂其囊皮完全由天然聚合物组成,可完全生物降解,因而无残留,可在无公害绿色经济作物上广泛使用。Compared with the prior art, a kind of nicotine microcapsule suspoemulsion of the present invention and its preparation method have substantive characteristics and remarkable progress: 1. The nicotine microcapsule suspoemulsion decomposes slowly when exposed to light, thereby improving its drug efficacy , at the same time prolong the drug effect time, it is known through the test that its original drug is reduced by 30-50%, the control effect is improved by 10-20%, and the duration of effect is extended by 3-10 times; Composed of natural polymers, it is completely biodegradable, so there is no residue, and can be widely used in pollution-free green economic crops.

(四)具体实施方式:(4) Specific implementation methods:

为了更好地理解与实施,下面结合实施例详细说明本发明一种烟碱微胶囊悬乳剂及其制备方法。For better understanding and implementation, a nicotine microcapsule suspoemulsion of the present invention and its preparation method will be described in detail below in conjunction with examples.

实施例1,将2.8g油状液烟碱、加入0.5g十二烷基苯磺酸钙、0.5g苯乙基酚聚氧乙烯聚氧丙烯醚、3g蓖麻油、4g三苯乙基酚聚氧乙烯醚、6g二甲苯,加热至70℃,同时不断进行搅拌,再加入16g水,备用;将8g明胶、8g褐藻酸钠分别加入92g水进行水解,分别加热至70℃,取上述水解后的胶液各25g进行过滤,过滤后混合,并搅拌均匀,将搅拌均匀的胶液加入前面制成的备用液中,在400转/分的转速下混合搅拌,同时自然降温2小时后,即得烟碱微胶囊悬乳剂。Example 1, add 2.8g oily liquid nicotine, add 0.5g calcium dodecylbenzenesulfonate, 0.5g styrylphenol polyoxyethylene polyoxypropylene ether, 3g castor oil, 4g tristyrylphenol polyoxygenate Vinyl ether and 6g xylene were heated to 70°C while stirring continuously, and then 16g of water was added for later use; 8g of gelatin and 8g of sodium alginate were added to 92g of water for hydrolysis, respectively, heated to 70°C, and the above-mentioned hydrolyzed Each 25g of the glue solution is filtered, mixed after filtering, and stirred evenly, and the well-stirred glue solution is added to the standby liquid prepared above, mixed and stirred at a speed of 400 rpm, and cooled naturally for 2 hours at the same time to obtain Nicotine microcapsule suspoemulsion.

上述实施例的烟碱微胶囊悬乳剂与5%的烟碱乳油在防治莱青虫药效持效期对比表如表1。Table 1 shows the comparison of the duration of efficacy of the nicotine microcapsule suspoemulsion and 5% nicotine emulsifiable concentrate in the control of Laibidia spp.

表1Table 1

  试验样 test sample 稀释倍数Dilution factor 药前虫数数头/株The number of pre-drug worms per plant      药前1天 1 day before the medicine        药后3天   3 days after taking the medicine         药后5天 5 days after the medicine   头/株 head/plant   校正防效% Correction effect %   头/株 head/plant   校正防效% Correction effect %   头/株 head/plant   校正防效% Correction effect %   烟碱微胶囊悬乳剂 Nicotine microcapsule suspoemulsion   1000 1000   8 8   1 1   87.5 87.5   1.2 1.2   80 80   2.5 2.5   68.75 68.75   5%烟碱乳油 5% Nicotine EC   1000 1000   6 6   2 2   66.7 66.7   7 7   0 0   7 7   0 0   对照组 control group   不施药 Do not apply   5 5   5 5   / /   6 6   / /   8 8   / /

实施例2,将5g油状液烟碱、加入0.6g十二烷基苯磺酸钙、0.6g蓖麻油环氧乙烷加成物、4g棉籽油、4.5g二苄基联苯酚聚氧乙烯醚、7g二甲苯,加热至60℃,同时不断进行搅拌,再加入18g水,备用;将8g淀粉胶、8g褐藻酸钠分别加入92g水进行水解,分别加热至60℃,取上述水解后的胶液各28g进行过滤,过滤后混合,并搅拌均匀,将搅拌均匀的胶液加入前面制成的备用液中,在500转/分的转速下混合搅拌,同时自然降温2小时后,即得烟碱微胶囊悬乳剂。Example 2, add 5g oily liquid nicotine, add 0.6g calcium dodecylbenzenesulfonate, 0.6g castor oil ethylene oxide adduct, 4g cottonseed oil, 4.5g dibenzyl biphenol polyoxyethylene ether , 7g of xylene, heated to 60°C while stirring continuously, then added 18g of water, and set aside; respectively added 8g of starch glue and 8g of sodium alginate to 92g of water for hydrolysis, heated to 60°C respectively, and took the above-mentioned hydrolyzed glue Filter each 28g of liquid, mix after filtering, and stir evenly, add the uniformly stirred glue liquid into the spare liquid prepared above, mix and stir at a speed of 500 rpm, and cool down naturally for 2 hours at the same time to obtain smoke Alkaline microcapsule suspoemulsion.

实施例3,将2g油状液烟碱、加入0.2g十二烷基苯磺酸钙、0.2g苯乙基酚聚氧乙烯聚氧丙烯醚、2g菜籽油、3g三苯乙基酚聚氧乙烯醚、5g二甲苯,加热至50℃,同时不断进行搅拌,再加入14g水,备用;将7.5g明胶、7.5g淀粉胶分别加入92g水进行水解,分别加热至50℃,取上述水解后的胶液各15g进行过滤,过滤后混合,并搅拌均匀,加入1g发泡剂,将搅拌均匀的胶液加入前面制成的备用液中,在200转/分的转速下混合搅拌,同时自然降温2小时后,即得烟碱微胶囊悬乳剂。Example 3, add 2g oily liquid nicotine, add 0.2g calcium dodecylbenzenesulfonate, 0.2g styrylphenol polyoxyethylene polyoxypropylene ether, 2g rapeseed oil, 3g tristyrylphenol polyoxygenate Vinyl ether and 5g xylene were heated to 50°C while stirring continuously, and then 14g of water was added for later use; 7.5g of gelatin and 7.5g of starch glue were respectively added to 92g of water for hydrolysis, respectively heated to 50°C, and the above hydrolyzed Each 15g of the glue solution is filtered, mixed after filtering, and stirred evenly, and 1g of foaming agent is added, and the well-stirred glue solution is added to the standby liquid prepared above, mixed and stirred at a speed of 200 rpm, and naturally After cooling down for 2 hours, the nicotine microcapsule suspoemulsion was obtained.

实施例4,将10g油状液烟碱、加入1g十二烷基苯磺酸钙、1g苯乙基酚聚氧乙烯聚氧丙烯醚、5g蓖麻油、5g三苯乙基酚聚氧乙烯醚、10g二甲苯,加热至80℃,同时不断进行搅拌,再加入20g水,备用;将8g明胶、8g褐藻酸钠分别加入92g水进行水解,分别加热至60℃,取上述水解后的胶液各30g进行过滤,过滤后混合,并搅拌均匀,将搅拌均匀的胶液加入前面制成的备用液中,在600转/分的转速下混合搅拌,同时自然降温2小时后,加入防冻液、染料后进行包装,即得烟碱微胶囊悬乳剂。Example 4, add 10g oily liquid nicotine, add 1g calcium dodecylbenzenesulfonate, 1g styrylphenol polyoxyethylene polyoxypropylene ether, 5g castor oil, 5g tristyrylphenol polyoxyethylene ether, Heat 10g of xylene to 80°C while stirring continuously, then add 20g of water and set aside; add 8g of gelatin and 8g of sodium alginate to 92g of water for hydrolysis, heat to 60°C respectively, and take the above hydrolyzed glue solution 30g to filter, filter and mix, and stir evenly, add the well-stirred glue solution to the spare solution prepared above, mix and stir at a speed of 600 rpm, and cool down naturally for 2 hours, then add antifreeze and dye After packing, the nicotine microcapsule suspoemulsion is obtained.

Claims (2)

1、烟碱微胶囊悬乳剂,其特征在于它是以烟碱为有效成份,并含有表面活性剂、植物油、助剂、溶剂、水,同时还含有海产品胶与动物胶和植物胶中的一种或两种的水解物的组合物;表面活性剂为三苯乙基酚聚氧乙烯醚、二苄基联苯酚聚氧乙烯醚,植物油为棉籽油、菜籽油、蓖麻油酸,助剂为十二烷基苯磺酸钙、苯乙基酚聚氧乙烯聚氧丙烯醚、蓖麻油环氧乙烷加成物,溶剂为二甲苯,动物胶为明胶,植物胶为淀粉胶,海产品胶为鱼胶、褐藻酸钠。1. Nicotine microcapsule suspoemulsion is characterized in that it takes nicotine as an active ingredient, and contains surfactants, vegetable oils, auxiliary agents, solvents, water, and also contains seafood glue, animal glue and vegetable glue. The composition of one or two kinds of hydrolyzate; Surfactant is tristyrylphenol polyoxyethylene ether, dibenzyl biphenol polyoxyethylene ether, vegetable oil is cottonseed oil, rapeseed oil, ricinoleic acid, helps The agent is calcium dodecylbenzenesulfonate, phenylethylphenol polyoxyethylene polyoxypropylene ether, castor oil ethylene oxide adduct, the solvent is xylene, the animal glue is gelatin, the vegetable glue is starch glue, sea The product glue is isinglass and sodium alginate. 2、权利要求1所述的烟碱微胶囊悬乳剂的制备方法,包括如下工艺步骤:2. The preparation method of the nicotine microcapsule suspoemulsion according to claim 1, comprising the following process steps: a,囊核的制作,将油状液烟碱中,加入助剂、植物油、表面活性剂,再加入溶剂进行稀释,加热至60-80℃,同时不断搅拌,再加入一定量的水;助剂为十二烷基苯磺酸钙、苯乙基酚聚氧乙烯聚氧丙烯醚、蓖麻油环氧乙烷加成物,植物油为棉籽油、菜籽油、蓖麻油酸,表面活性剂为三苯乙基酚聚氧乙烯醚、二苄基联苯酚聚氧乙烯醚,溶剂为二甲苯;a, the production of the capsule core, adding additives, vegetable oil, and surfactant to the oily liquid nicotine, then adding a solvent to dilute, heating to 60-80°C, stirring continuously at the same time, and then adding a certain amount of water; additives Calcium dodecylbenzenesulfonate, phenylethylphenol polyoxyethylene polyoxypropylene ether, castor oil ethylene oxide adduct, vegetable oil is cottonseed oil, rapeseed oil, ricinoleic acid, surfactant is three Phenylphenol polyoxyethylene ether, dibenzyl biphenol polyoxyethylene ether, the solvent is xylene; b,囊皮的制作,将海产品胶与动物胶和植物胶中的一种或两种胶分别先进行各类胶的水解,分别加热至60-80℃,过滤后混合,搅拌均匀即可;海产品胶为鱼胶、褐藻酸钠,动物胶为明胶,植物胶为淀粉胶;b. For the production of capsule skin, hydrolyze seafood glue, one or two kinds of glue from animal glue and vegetable glue, respectively, heat them to 60-80°C, filter and mix, and stir evenly. The seafood glue is isinglass and sodium alginate, the animal glue is gelatin, and the vegetable glue is starch glue; c,微胶囊制剂,将步骤b的囊皮原料倒入步骤a的囊核的反应釜中,在300-600转/分的转速下混合搅拌,同时自然降温2小时后,进行包装。c, microcapsule preparation, pour the raw material of capsule skin in step b into the reaction kettle of capsule core in step a, mix and stir at a speed of 300-600 rpm, and pack after natural cooling for 2 hours.
CN 03139131 2003-08-16 2003-08-16 Nicotine microcapsule suspoemulsion and preparation method thereof Expired - Fee Related CN1229020C (en)

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CN103651588B (en) * 2013-09-10 2015-11-11 北京联合大学生物化学工程学院 A kind of preparation method of the encapsulate pesticides for killing aphid
CN110250174B (en) * 2018-03-12 2022-08-19 侨昌现代农业有限公司 Oil-containing dry suspending agent formulation and processing technology thereof
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