Synthesis method of ketazine

A technique for the synthesis of acetonazine, which is applied in the preparation of hydrazone, organic chemistry, etc., can solve the problems of increasing the production cost of hydrazine hydrate, reducing the yield of synthetic ketazine, and increasing the side reactions in the hydrolysis process, etc., so as to reduce the processing frequency and Effects of steam energy consumption, reduction of processing capacity, and suppression of side reactions

Active Publication Date: 2015-08-26
杭州圣捷菲科技有限公司
View PDF4 Cites 3 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the accumulation of impurities, the yield of synthetic ketazine is gradually reduced. At the same time, the isopropanol impurity will cause an increase in the side reactions of the hydrolysis process after entering the hydrolysis tower with the ketazine, thereby reducing the yield of hydrazine hydrate.
In order to control the isopropanol content in the reaction system below 1%, usually when the isopropanol content in the recovered acetone reaches 8%, the recovered acetone needs to be distilled and purified. A large amount of steam will be consumed in the process, and a large amount of waste water containing IPA will be generated, which will increase the production cost of hydrazine hydrate

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Add 370mL of water, 441.6mL of acetone, and 0.10g of gelatin into the reactor equipped with agitator, thermometer, ammonia gas introduction tube and reflux condenser, heat and stir, and inject ammonia gas after the gelatin is dissolved until it is saturated (the liquid level has After the gas overflows), it is changed to slow feeding, and when the temperature is raised to 50°C, 1128g of 13.2% sodium hypochlorite aqueous solution is slowly added dropwise, and the dripping is completed in 1.5h, and the temperature is controlled at 50~60°C to continue the reaction for 1.5h. After the reaction is over, transfer the reaction liquid to a distillation device, heat up, and distill out low boiling substances such as acetonazine, acetone, and isopropanol in the reaction liquid, condense and recover, and stop distillation when the temperature of the distillation port reaches 96°C , carry out content analysis after weighing the condensate sample. The calculated yield of acetonazine...

Embodiment 2

[0035]Add 297mL of water, 386.4mL of acetone, and 0.15g of xanthan gum into the reactor equipped with agitator, thermometer, ammonia gas introduction tube, and reflux condenser, heat and stir, and inject ammonia gas after the xanthan gum dissolves until saturated (Gas overflowed from the liquid surface) After that, it was changed to slow feeding, and when the temperature was raised to 51°C, 852.4g of 13.1% sodium hypochlorite aqueous solution was slowly added dropwise, and the dripping was completed in 2 hours. After the reaction is over, transfer the reaction liquid to a distillation device, heat up, and distill out low boiling substances such as acetonazine, acetone, and isopropanol in the reaction liquid, condense and recover, and stop distillation when the temperature of the distillation port reaches 96°C , weigh the condensate sample and analyze the content of the material. The calculated yield of acetonazine is 97.6%, and the production amount of isopropanol is 0.0012mol...

Embodiment 3

[0037] Add water 490mL, acetone 736mL, and guar gum 0.20g to the reactor equipped with stirring, thermometer, ammonia inlet pipe, and reflux condenser, heat and stir, and feed ammonia gas after the guar gum dissolves until saturated ( There is gas overflow on the liquid surface) after that, it was changed to slow feeding, and when the temperature was raised to 53 °C, 1399.2 g of 13.3% sodium hypochlorite aqueous solution was slowly added dropwise, and the dripping was completed in 1.5 hours, and the temperature was controlled at 50-60 °C to continue the reaction for 1.5 h. After the reaction is over, transfer the reaction liquid to a distillation device, heat up, and distill out low boiling substances such as acetonazine, acetone, and isopropanol in the reaction liquid, condense and recover, and stop distillation when the temperature of the distillation port reaches 96°C , weigh the condensate and analyze the content of the material. The calculated yield of acetonazine is 97.9...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

No PUM Login to view more

Abstract

The invention belongs to the chemical field of chemical synthesis, and particularly relates to a synthesis method of ketazine. The ynthesis method can restrain side reaction, reduce the generation of side reaction products and deleterious impurities, improve the yield of ketazine and reduce energy consumption. The synthesis method adopts the technical scheme that acetone and ammonia are taken as raw materials, sodium hypochlorite is taken as an oxidizing agent, so as to synthesize ketazine. The synthesis method is characterized in that a side-reaction inhibitor is added in a reaction system. The side-reaction inhibitor can be one or more of gelatin, xanthan gum, guar gum and sodium acetylide. The synthesis method can effectively restrain the occurrence of side reaction, and improves the yield of ketazine from 90-91 percent to 97-98 percent, reduces the treatment frequency for acetone distillation and purification (for removing side reaction product isopropanol) and steam consumption, reduces the handling capacity of isopropanol wastewater, and lowers the production cost.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and in particular relates to a synthesis method of acetonazine. Background technique [0002] Acetonazine is an important intermediate for the preparation of hydrazine hydrate. As we all know, hydrazine hydrate is an important chemical raw material and has a wide range of uses. Since the hydrazine hydrate molecule contains two nucleophilic nitrogens and four replaceable hydrogens, the fine chemical products using hydrazine hydrate as raw materials involve almost all fields. . Therefore, improving the production process of hydrazine hydrate and ketazine, increasing their yield, and reducing production costs have always been the focus of people's research. [0003] At present, there are three main production process routes of hydrazine hydrate in China. The first is the Rasch method, which is an ancient method for producing hydrazine in industry. It uses ammonia as a raw material and ...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
Patent Type & Authority Applications(China)
IPC IPC(8): C07C251/88C07C249/16
Inventor 李亚杉
Owner 杭州圣捷菲科技有限公司
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap