CN105646623A - Emamectin benzoate amination reaction dichloromethane instead of isopropyl acetate and process method thereof - Google Patents
Emamectin benzoate amination reaction dichloromethane instead of isopropyl acetate and process method thereof Download PDFInfo
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- CN105646623A CN105646623A CN201410672818.8A CN201410672818A CN105646623A CN 105646623 A CN105646623 A CN 105646623A CN 201410672818 A CN201410672818 A CN 201410672818A CN 105646623 A CN105646623 A CN 105646623A
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- methylene dichloride
- isopropyl acetate
- amination reaction
- emamectin benzoate
- dichloromethane
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Abstract
An emamectin benzoate amination reaction dichloromethane instead of isopropyl acetate and a process method thereof are provided. According to oxides of avermectin, dichloromethane, heptamethyldisilazane and zinc trifluoroacetate as raw materials are processed according to a certain weight ratio to prepare a product. With dichloromethane instead of isopropyl acetate, through multiple replication of a lot of experiments, equipment has no need for large change, the content of the product is high, the yield can be guaranteed, the price is low, the cost of each batch of raw materials can be reduced by 2704 yuan, moreover, the used dichloromethane is not inflammable and explosive, and the safe production of enterprises can be guaranteed. In addition, dichloromethane after disposable use can be recycled and reused, the recycling process is convenient and easy, the raw materials are saved, and popularization and application are facilitated.
Description
Technical field: the present invention relates to a kind of emamectin benzoate amination reaction methylene dichloride and replace isopropyl acetate and processing method thereof.
Background technology: at present, emamectin benzoate amination reaction uses isopropyl acetate to make solvent, its product price height, inflammable and explosive, run into naked light and easily explode, dangerous big, safety coefficient is low, in addition, and isopropyl acetate recycling difficulty, cannot be recycled after single use, waste raw material.
Summary of the invention: it is an object of the invention to overcome above-mentioned shortcoming, it is provided that a kind of emamectin benzoate amination reaction methylene dichloride replaces isopropyl acetate and processing method thereof, and its product price is low, and content receipts rate height, can be recycled after single use, nonflammable explosive. The object of the present invention is achieved like this, calculates with the oxide compound of 150kg Avrmectin, and methylene dichloride 150-250kg, heptamethyldisilazane 50-70kg, mass concentration are the trifluoroacetic acid zinc 50-70kg of 17%. Its processing method be the oxide compound of 150kg Avrmectin is taken off molten clean after; amination reaction first adds 50-100kg methylene dichloride in 1000L reactor and makees solvent; add 50-70kg heptamethyldisilazane again; stir after melting; add the trifluoroacetic acid zinc 50-70kg that mass concentration is 17%; stir; it is warming up to 50-55 DEG C; react 2-3 hour; condenser keeps backflow, sampling analysis, is qualified within oxide compound residue 2.5%; cool to 40 DEG C and add the dilution of 100-150kg methylene dichloride again, cross and expect deprotection still. This invention replaces isopropyl acetate with methylene dichloride, and through repeatedly repeatedly testing in a large number, equipment is without the need to big variation, product content height, receipts rate can be ensured, price is low, often criticize raw material and can reduce costs 2704 yuan, and the methylene dichloride used is nonflammable explosive, the safety in production of enterprise can be protected, in addition, recyclable recycling after methylene dichloride single use, recovery process is easily convenient, saves material, is conducive to applying.
Specific embodiment:
Embodiment 1: most preferred embodiment
Calculating with the oxide compound of 150kg Avrmectin, methylene dichloride 200kg, heptamethyldisilazane 60kg, mass concentration are the trifluoroacetic acid zinc 60kg of 17%.Its processing method be the oxide compound of 150kg Avrmectin is taken off molten clean after, amination reaction first adds 65kg methylene dichloride in 1000L reactor and makees solvent, then adds 60kg heptamethyldisilazane; stir after melting; add the trifluoroacetic acid zinc 60kg that mass concentration is 17%, stir, be warming up to 50-55 DEG C; react 2 hours; condenser keeps backflow, sampling analysis, is qualified within oxide compound residue 2.5%; cool to 40 DEG C and add the dilution of 135kg methylene dichloride again, cross and expect deprotection still.
Embodiment 2:
Calculating with the oxide compound of 150kg Avrmectin, methylene dichloride 150kg, heptamethyldisilazane 50kg, mass concentration are the trifluoroacetic acid zinc 50kg of 17%. Its processing method be the oxide compound of 150kg Avrmectin is taken off molten clean after, amination reaction first adds 50kg methylene dichloride in 1000L reactor and makees solvent, then adds 50kg heptamethyldisilazane; stir after melting; add the trifluoroacetic acid zinc 50kg that mass concentration is 17%, stir, be warming up to 50-55 DEG C; react 3 hours; condenser keeps backflow, sampling analysis, is qualified within oxide compound residue 2.5%; cool to 40 DEG C and add the dilution of 100kg methylene dichloride again, cross and expect deprotection still.
Embodiment 3:
Calculating with the oxide compound of 150kg Avrmectin, methylene dichloride 250kg, heptamethyldisilazane 70kg, mass concentration are the trifluoroacetic acid zinc 70kg of 17%. Its processing method be the oxide compound of 150kg Avrmectin is taken off molten clean after, amination reaction first adds 100kg methylene dichloride in 1000L reactor and makees solvent, then adds 70kg heptamethyldisilazane; stir after melting; add the trifluoroacetic acid zinc 70kg that mass concentration is 17%, stir, be warming up to 50-55 DEG C; react 3 hours; condenser keeps backflow, sampling analysis, is qualified within oxide compound residue 2.5%; cool to 40 DEG C and add the dilution of 150kg methylene dichloride again, cross and expect deprotection still.
Claims (2)
1. an emamectin benzoate amination reaction methylene dichloride replaces isopropyl acetate, it is characterized in that: calculate with the oxide compound of 150kg Avrmectin, methylene dichloride 150-250kg, heptamethyldisilazane 50-70kg, mass concentration are the trifluoroacetic acid zinc 50-70kg of 17%.
2. emamectin benzoate amination reaction methylene dichloride according to claim 1 replaces the processing method of isopropyl acetate, it is characterized in that: the oxide compound of 150kg Avrmectin is taken off molten clean after, amination reaction first adds 50-100kg methylene dichloride in 1000L reactor and makees solvent, add 50-70kg heptamethyldisilazane again, stir after melting, add the trifluoroacetic acid zinc 50-70kg that mass concentration is 17%, stir, it is warming up to 50-55 DEG C, react 2-3 hour, condenser keeps backflow, sampling analysis, it is qualified within oxide compound residue 2.5%, cool to 40 DEG C and add the dilution of 100-150kg methylene dichloride again, cross and expect deprotection still.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410672818.8A CN105646623A (en) | 2014-11-23 | 2014-11-23 | Emamectin benzoate amination reaction dichloromethane instead of isopropyl acetate and process method thereof |
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| CN201410672818.8A CN105646623A (en) | 2014-11-23 | 2014-11-23 | Emamectin benzoate amination reaction dichloromethane instead of isopropyl acetate and process method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111256975A (en) * | 2020-03-10 | 2020-06-09 | 郑州赛奥电子股份有限公司 | Device and method for checking opening time of pressure release valve |
| CN112707810A (en) * | 2020-12-24 | 2021-04-27 | 内蒙古新威远生物化工有限公司 | Preparation method of zinc trifluoroacetate and application of zinc trifluoroacetate in emamectin benzoate production |
| CN116237084A (en) * | 2022-12-10 | 2023-06-09 | 河北兴柏农业科技股份有限公司 | Supported zinc trifluoroacetate, preparation method and application |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103012525A (en) * | 2013-01-05 | 2013-04-03 | 哈尔滨理工大学 | Method for synthesizing emamectin benzoate |
| CN103408622A (en) * | 2013-08-22 | 2013-11-27 | 河北美荷药业有限公司 | Synthesis method of emamectin benzoate |
-
2014
- 2014-11-23 CN CN201410672818.8A patent/CN105646623A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103012525A (en) * | 2013-01-05 | 2013-04-03 | 哈尔滨理工大学 | Method for synthesizing emamectin benzoate |
| CN103408622A (en) * | 2013-08-22 | 2013-11-27 | 河北美荷药业有限公司 | Synthesis method of emamectin benzoate |
Non-Patent Citations (2)
| Title |
|---|
| 喻艳超: "甲胺基阿维菌素苯甲酸盐合成工艺研究", 《哈尔滨理工大学硕士学位论文》 * |
| 汪桂颖: "影响甲氨基阿维菌素苯甲酸盐合成过程中胺化反应速度的因素探讨", 《化学工程师》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111256975A (en) * | 2020-03-10 | 2020-06-09 | 郑州赛奥电子股份有限公司 | Device and method for checking opening time of pressure release valve |
| CN112707810A (en) * | 2020-12-24 | 2021-04-27 | 内蒙古新威远生物化工有限公司 | Preparation method of zinc trifluoroacetate and application of zinc trifluoroacetate in emamectin benzoate production |
| CN116237084A (en) * | 2022-12-10 | 2023-06-09 | 河北兴柏农业科技股份有限公司 | Supported zinc trifluoroacetate, preparation method and application |
| CN116237084B (en) * | 2022-12-10 | 2024-06-07 | 河北兴柏农业科技股份有限公司 | Supported zinc trifluoroacetate, preparation method and application |
| WO2024119657A1 (en) * | 2022-12-10 | 2024-06-13 | 河北兴柏农业科技股份有限公司 | Supported zinc trifluoroacetate, preparation method and use |
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Application publication date: 20160608 |