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CN103168783B - Azadirachtin emulsion composition and preparation method of azadirachtin emulsion composition - Google Patents

Azadirachtin emulsion composition and preparation method of azadirachtin emulsion composition Download PDF

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CN103168783B
CN103168783B CN201110434202.3A CN201110434202A CN103168783B CN 103168783 B CN103168783 B CN 103168783B CN 201110434202 A CN201110434202 A CN 201110434202A CN 103168783 B CN103168783 B CN 103168783B
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azadirachtin
emulsifier
antifreeze
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CN103168783A (en
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丁城峰
李富根
刘艳
黄耿
吴学民
张勇
朱新成
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Chengdu Lyujin Biological Science & Technology Co ltd
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Chengdu Greengold High Tech Co ltd
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Abstract

印楝素乳油组合物及其制备方法。该印楝素乳油组合物,由印楝素、乳化剂、渗透剂、稳定剂、抗冻剂、助溶剂和溶剂组成,其中各组分的含量(重量)为:印楝素:0.3%-1%;乳化剂:8%-12%;渗透剂:5%-8%;稳定剂:5%-10%;抗冻剂:5%-10%;助溶剂:5%-10%;溶剂:余量。本发明的印楝素乳油组合物由于其组分之间的相互协同效应,能够使印楝素得以充分溶解。另外,由于采用了植物油溶剂,从而大大减小了溶剂毒性,使所得制剂更加环保安全。Azadirachtin emulsifiable oil composition and preparation method thereof. The azadirachtin emulsifiable oil composition is composed of azadirachtin, emulsifier, penetrant, stabilizer, antifreeze agent, cosolvent and solvent, wherein the content (weight) of each component is: azadirachtin: 0.3%- 1%; Emulsifier: 8%-12%; Penetrant: 5%-8%; Stabilizer: 5%-10%; Antifreeze: 5%-10%; Co-solvent: 5%-10%; Solvent :margin. The azadirachtin emulsifiable oil composition of the present invention can fully dissolve the azadirachtin due to the synergistic effect among its components. In addition, since the vegetable oil solvent is used, the toxicity of the solvent is greatly reduced, and the obtained preparation is more environmentally friendly and safe.

Description

印楝素乳油组合物及其制备方法Azadirachtin emulsifiable oil composition and preparation method thereof

技术领域 technical field

本发明涉及印楝素乳油组合物及其制备方法。  The invention relates to azadirachtin emulsifiable oil composition and a preparation method thereof. the

背景技术 Background technique

乳油是由不溶于水的原药、有机溶剂苯、二甲苯等和乳化剂配置加工而成的透明状液体,常温下密封存放两年一般不会浑浊、分层和沉淀,加入水中迅速均匀分散成不透明的乳状液。乳油的特点是:药效高,施用方便,性质较稳定。由于乳油的历史较长,具有成熟的加工技术,所以品种多,产量大,应用范围广,目前仍然是农药的一个主要剂型,但是其在使用中存在着很大问题。  The emulsifiable concentrate is a transparent liquid processed from water-insoluble raw materials, organic solvents such as benzene and xylene, and emulsifiers. It will not be turbid, stratified, or precipitated after being sealed and stored at room temperature for two years. It can be quickly and evenly dispersed when added to water. into an opaque emulsion. The characteristics of the emulsifiable concentrate are: high drug efficacy, convenient application and relatively stable properties. Due to its long history and mature processing technology, EC has many varieties, large output and wide application range. It is still a main dosage form of pesticides, but there are big problems in its use. the

乳油问题的关键是溶剂,目前我国乳油所使用的溶剂主要是易挥发轻芳烃溶剂,该溶剂具有毒性较高、易燃、半衰期长、对环境影响大等缺点。此外,在其他一些剂型中还使用较多的毒性较高或具有致畸性的溶剂,如甲醇、二甲基甲酰胺等,因此,如果能使用相对毒性较低、安全性较高的溶剂,乳油仍是一种好的剂型。  The key to the EC problem is the solvent. At present, the solvents used in my country's EC are mainly volatile light aromatic solvents, which have the disadvantages of high toxicity, flammability, long half-life, and great impact on the environment. In addition, more toxic or teratogenic solvents, such as methanol and dimethylformamide, are used in some other dosage forms. Therefore, if solvents with relatively low toxicity and high safety can be used, Cream is still a good dosage form. the

印楝素乳油是采用乳油剂型的一种农药,其中印楝素是一种有多种毒杀害虫作用的植物源活性物质,存在于印楝属印楝植物种核和叶子中。印楝素由于在水中易分解水基化产品开发难度较大,目前乳油仍将是印楝素的主要剂型。因此,如何对印楝素乳油的剂型进行优化,特别是如何对乳油中各种助剂剂型进行改良,使印楝素制剂更环保安全,是亟待解决的技术问题。  Azadirachtin EC is a pesticide in the form of an emulsifiable concentrate, in which azadirachtin is a plant-derived active substance with multiple poisoning and insecticidal effects, and exists in the seeds and leaves of the neem plant of the genus Azadirachta. Because azadirachtin is easily decomposed in water, it is difficult to develop water-based products. At present, EC will still be the main dosage form of azadirachtin. Therefore, how to optimize the dosage form of azadirachtin emulsifiable concentrate, especially how to improve the dosage forms of various additives in the emulsifiable concentrate, so as to make the azadirachtin preparation more environmentally friendly and safe, is a technical problem to be solved urgently. the

发明内容 Contents of the invention

本发明的目的是提供一种更加环保安全的印楝素乳油组合物。  The purpose of the present invention is to provide a more environmentally safe azadirachtin emulsifiable oil composition. the

根据本发明的第一方面,提供了一种印楝素乳油组合物。该组合物由印楝素、乳化剂、渗透剂、稳定剂、抗冻剂、助溶剂和溶剂组成,其中各组分的含量(重量)如下:  According to the first aspect of the present invention, an azadirachtin emulsifiable oil composition is provided. The composition is made up of azadirachtin, emulsifier, penetrant, stabilizer, antifreeze, cosolvent and solvent, wherein the content (weight) of each component is as follows:

印楝素:0.3%-1%;乳化剂:8%-12%;渗透剂:5%-8%;稳定剂:5%-10%;抗冻剂:5%-10%;助溶剂:5%-10%;溶剂:余量。  Azadirachtin: 0.3%-1%; Emulsifier: 8%-12%; Penetrant: 5%-8%; Stabilizer: 5%-10%; Antifreeze: 5%-10%; Cosolvent: 5%-10%; solvent: balance. the

溶剂可以选自桉油、松脂基植物油、印楝油和小桐子油等植物油。  The solvent may be selected from vegetable oils such as eucalyptus oil, turpentine-based vegetable oil, neem oil, and jatropha oil. the

乳化剂可以选自失水山梨醇单硬脂酸酯、聚氧乙烯失水山梨醇醚 单油酸酯和脂肪醇聚氧乙烯醚。  The emulsifier may be selected from sorbitan monostearate, polyoxyethylene sorbitan monooleate and fatty alcohol polyoxyethylene ethers. the

渗透剂可以选自NP类非离子表面活性剂、AEO类非离子表面活性剂和有机硅。  The penetrant may be selected from NP-type nonionic surfactants, AEO-type nonionic surfactants, and silicones. the

稳定剂可以选自2,6二叔丁基对甲酚、山梨酸、聚乙烯基乙二醇缩水甘油醚、甲苯基缩水甘油醚,丁基缩水甘油醚和双(2,2,6,6-四甲基哌啶基)癸二酸酯。  Stabilizer can be selected from 2,6 di-tert-butyl p-cresol, sorbic acid, polyvinyl glycol glycidyl ether, cresyl glycidyl ether, butyl glycidyl ether and bis(2,2,6,6 - tetramethylpiperidinyl) sebacate. the

抗冻剂可以选自乙二醇、丙三醇和山梨醇。  The antifreeze agent may be selected from ethylene glycol, glycerol and sorbitol. the

助溶剂可以选自乙醇和二价酸酯。  Co-solvents can be selected from ethanol and dibasic acid esters. the

根据本发明的另一方面,提供了上述印楝素乳油组合物的制备方法。该方法包括:  According to another aspect of the present invention, a preparation method of the above-mentioned azadirachtin cream composition is provided. The method includes:

用助溶剂充分溶解印楝素;  Fully dissolve azadirachtin with a cosolvent;

然后加入乳化剂和溶剂总量的1/3进行充分乳化;  Then add 1/3 of the total amount of emulsifier and solvent to fully emulsify;

再加入抗冻剂和稳定剂并搅拌混合均匀;以及  Then add the antifreeze and stabilizer and mix well; and

最后加入其余的溶剂并进行搅拌。  Finally the rest of the solvent was added and stirred. the

通过本发明的方法所制备的印楝素乳油组合物,由于其组分之间的相互协同效应,从而使印楝素能够得以充分溶解。另外,由于采用了植物油溶剂,从而大大减小了溶剂毒性,使所得制剂更加环保安全。  The azadirachtin emulsifiable oil composition prepared by the method of the invention can fully dissolve the azadirachtin due to the synergistic effect among its components. In addition, since the vegetable oil solvent is used, the toxicity of the solvent is greatly reduced, and the obtained preparation is more environmentally friendly and safe. the

具体实施方式 Detailed ways

下面结合具体实施例详细描述本发明的印楝素乳油组合物及其制备方法。  The azadirachtin emulsifiable oil composition of the present invention and its preparation method are described in detail below in conjunction with specific examples. the

本发明的印楝素乳油组合物由印楝素、乳化剂、渗透剂、稳定剂、抗冻剂、助溶剂和溶剂组成,其制备方法如下:  Azadirachtin emulsifiable oil composition of the present invention is made up of azadirachtin, emulsifier, penetrating agent, stabilizer, antifreeze agent, cosolvent and solvent, and its preparation method is as follows:

用助溶剂充分溶解印楝素;  Fully dissolve azadirachtin with a cosolvent;

然后加入乳化剂和溶剂总量的1/3进行充分乳化;  Then add 1/3 of the total amount of emulsifier and solvent to fully emulsify;

再加入抗冻剂和稳定剂并搅拌混合均匀;以及  Then add the antifreeze and stabilizer and mix well; and

最后加入其余的溶剂并进行搅拌0.5小时-1小时。  Finally the rest of the solvent was added and stirring was carried out for 0.5-1 hour. the

下面给出本发明的印楝素乳油组合物的几个具体实施例。  Several specific examples of the azadirachtin emulsifiable concentrate composition of the present invention are given below. the

印楝素乳油组合物1(各组分的比例为重量比)  Azadirachtin emulsifiable oil composition 1 (the ratio of each component is weight ratio)

印楝素:(0.3%);  Azadirachtin: (0.3%);

乳化剂:失水山梨醇单硬脂酸酯(8%);  Emulsifier: Sorbitan Monostearate (8%);

渗透剂:烷基酚聚氧乙烯醚(5%);  Penetrant: Alkylphenol polyoxyethylene ether (5%);

稳定剂:2,6二叔丁基对甲酚(5%);  Stabilizer: 2,6 di-tert-butyl-p-cresol (5%);

抗冻剂:乙二醇(5%);  Antifreeze: ethylene glycol (5%);

助溶剂:乙醇(5%);和  Co-solvent: ethanol (5%); and

溶剂:桉油(余量)。  Solvent: eucalyptus oil (balance). the

印楝素乳油组合物2(各组分的比例为重量比)  Azadirachtin emulsifiable oil composition 2 (the ratio of each component is weight ratio)

印楝素:(0.5%);  Azadirachtin: (0.5%);

乳化剂:聚氧乙烯失水山醇醚单油酸酯(10%);  Emulsifier: polyoxyethylene behenyl ether monooleate (10%);

渗透剂:有机硅(8%);  Penetrant: Silicone (8%);

稳定剂:山梨酸(8%);  Stabilizer: sorbic acid (8%);

抗冻剂:丙三醇(8%);  Antifreeze: glycerol (8%);

助溶剂:二价酸酯(10%);和  Co-solvent: dibasic acid ester (10%); and

溶剂:松脂基植物油(余量)。  Solvent: turpentine-based vegetable oil (balance). the

印楝素乳油组合物3(各组分的比例为重量比)  Azadirachtin emulsifiable oil composition 3 (the ratio of each component is weight ratio)

印楝素:(1%);  Azadirachtin: (1%);

乳化剂:脂肪醇聚氧乙烯醚(12%);  Emulsifier: fatty alcohol polyoxyethylene ether (12%);

渗透剂:烷基酚聚氧乙烯醚(5%);  Penetrant: Alkylphenol polyoxyethylene ether (5%);

稳定剂:甲苯基缩水甘油醚(10%);  Stabilizer: cresyl glycidyl ether (10%);

抗冻剂:山梨醇(10%);  Antifreeze: Sorbitol (10%);

助溶剂:乙醇(8%);以及  Co-solvent: ethanol (8%); and

溶剂:小桐子油(余量)。  Solvent: jatropha oil (remainder). the

本领域技术人员应当理解,上述具体实施例仅用于解释本发明而非用于对其作出任何限制。虽然本发明中使用的印楝素可以是提纯形式,但也可以采用其它形式例如含有印楝素有效成分的印楝粉或印楝素浸膏,只要最终制备的印楝素乳油组合物中所含的印楝素的重量含量在0.3%至1%之间即可。例如,上述印楝素乳油组合物1中重量比为3%的印楝素也可以由重量比为0.72%的印楝粉(该印楝粉含41%的印楝素有效活性成分)来替代提供。  It should be understood by those skilled in the art that the above specific embodiments are only used to explain the present invention and not to limit it in any way. Although the azadirachtin used in the present invention can be in a purified form, other forms such as azadirachtin powder or azadirachtin extract containing active ingredients of azadirachtin can also be used, as long as the final preparation of azadirachtin cream composition contains The weight content of the azadirachtin contained is between 0.3% and 1%. For example, in the above-mentioned azadirachtin emulsifiable oil composition 1, the weight ratio of 3% azadirachtin can also be replaced by 0.72% azadirachtin powder (this neem powder contains 41% azadirachtin active ingredient) supply. the

Claims (4)

1. a nimbin emulsion composition, the weight content of each component is as follows:
Nimbin: 0.3%; Emulsifier: 8%; Bleeding agent: 5%; Stabilizing agent: 5%; Antifreeze: 5%; Cosolvent: 5%; Solvent: surplus; Wherein
Emulsifier is sorbitan monostearate;
Bleeding agent is alkylphenol polyoxyethylene;
Stabilizing agent is 2,6 BHTs;
Antifreeze is ethylene glycol;
Cosolvent is ethanol;
Solvent is volatile oil extracted from eucalyptus' leaves or twigs.
2. a nimbin emulsion composition, the weight content of each component is as follows:
Nimbin: 0.5%; Emulsifier: 10%; Bleeding agent: 8%; Stabilizing agent: 8%; Antifreeze: 8%; Cosolvent: 10%; Solvent: surplus; Wherein
Emulsifier is polyoxyethylene dehydration mountain alcohol ether monoleate;
Bleeding agent is organosilicon;
Stabilizing agent is sorbic acid;
Antifreeze is glycerine;
Cosolvent is dibasic ester;
Solvent is turpentine-based vegetable oil.
3. a nimbin emulsion composition, the weight content of each component is as follows:
Nimbin: 1%; Emulsifier: 12%; Bleeding agent: 5%; Stabilizing agent: 10%; Antifreeze: 10%; Cosolvent: 8%; Solvent: surplus; Wherein
Emulsifier is fatty alcohol-polyoxyethylene ether;
Bleeding agent is alkylphenol polyoxyethylene;
Stabilizing agent is cresyl glycidyl ether;
Antifreeze is sorbierite;
Cosolvent is ethanol;
Solvent is Jatropha curcas oil.
4. according to the preparation method of the nimbin emulsion composition described in any one in claim 1-3, comprising:
Fully dissolve nimbin with cosolvent;
Then add 1/3 of emulsifier and solvent total amount to carry out fully emulsified;
Add again antifreeze and stabilizing agent and be uniformly mixed; And finally add remaining solvent and stir.
CN201110434202.3A 2011-12-22 2011-12-22 Azadirachtin emulsion composition and preparation method of azadirachtin emulsion composition Active CN103168783B (en)

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CN103766335A (en) * 2014-01-27 2014-05-07 崔建州 Grease and wax dissolving penetrating agent
CN104255747A (en) * 2014-09-02 2015-01-07 石家庄市青冠化工有限公司 Environment-friendly azadirachtin missible oil and preparation method thereof

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Inventor after: Ding Chengfeng

Inventor after: Li Fugen

Inventor after: Liu Yan

Inventor after: Huang Geng

Inventor after: Wu Xuemin

Inventor after: Zhang Yong

Inventor after: Zhu Xincheng

Inventor before: Ma Jianju

Inventor before: Huang Geng

Inventor before: Ding Chengfeng

Inventor before: Zhang Yong

Inventor before: Liu Yan

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Free format text: CORRECT: INVENTOR; FROM: MA JIANJU HUANG GENG DING CHENGFENG ZHANG YONG LIU YAN TO: DING CHENGFENG LI FUGEN LIU YAN HUANG GENG WU XUEMIN ZHANG YONG ZHU XINCHENG

C14 Grant of patent or utility model
GR01 Patent grant
C41 Transfer of patent application or patent right or utility model
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Effective date of registration: 20161228

Address after: 611500 Sichuan city of Chengdu province Qionglai city Linchiung fishing village (Linqiong Industrial Park) sing

Patentee after: CHENGDU LYUJIN BIOLOGICAL SCIENCE & TECHNOLOGY CO.,LTD.

Address before: High tech Zone Gaopeng road in Chengdu city of Sichuan province 610041 No. 5 Technology Innovation Service Center

Patentee before: CHENGDU GREENGOLD HIGH-TECH Co.,Ltd.

EE01 Entry into force of recordation of patent licensing contract

Application publication date: 20130626

Assignee: Sichuan Green Gold Biotechnology Co.,Ltd.

Assignor: CHENGDU LYUJIN BIOLOGICAL SCIENCE & TECHNOLOGY CO.,LTD.

Contract record no.: X2025510000009

Denomination of invention: Azadirachtin emulsion composition and its preparation method

Granted publication date: 20140903

License type: Common License

Record date: 20250312