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Preparation method of refined aziridine

A technology of aziridine and rectification, which is applied in the field of refined aziridine preparation, can solve the problems of time-consuming, energy-consuming, time-consuming and labor-consuming, and many by-products, and achieve the effect of reducing costs

Active Publication Date: 2022-04-29
上海健倬生物科技有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the synthetic methods of aziridine monomer mainly include sulfuric esterification method, 2-chloroethylamine method, dichloroethane method, ethylene oxide method and alkane amine gas phase dehydration method; Germany BASF mainly adopts monoethanolamine liquid phase method , while Nippon Catalyst uses the more advanced monoethanolamine gas phase method, the process is simple, but the catalyst is the core technology. At present, no other company has adopted the monoethanolamine gas phase method. The current domestic industrialization mainly adopts the monoethanolamine sulfation method; currently aziridine The purification all adopts the rectifying method, because the aziridine water content that prior art synthesizes is high (about 50%-80%), by-product is many, vacuum rectification is not only time-consuming and labor-intensive, single rectification nitrogen The purity of propidine is not high, so it can only be rectified many times, otherwise it will be difficult to meet the needs of fine chemical industry, medicine, aziridine cross-linking agent, etc.
[0003] The patent application number is: 201910296900.8 The purification of crude aziridine needs to be distilled at 45-95°C for 4-10 hours, repeated 3-5 times, and then the fraction at 20-60°C is collected under reduced pressure for 8-12 hours; The patent application number is: 201910196848.9 discloses a method for preparing methyl aziridine, wherein the refining process of methyl aziridine is similar to the patent application number: 201910296900.8, the method of purifying the product is time-consuming and energy-consuming, and the obtained The aziridine is not pure enough and the moisture content is too high

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  • Preparation method of refined aziridine
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  • Preparation method of refined aziridine

Examples

Experimental program
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Effect test

Embodiment 1

[0035] Preparation of crude aziridine: Accurately weigh 67g of monoethanolamine, add 108g of 98% concentrated sulfuric acid dropwise at room temperature, and finish dropping after 4 hours. , lower the temperature to 30°C, add 276g of sodium hydroxide aqueous solution with a mass concentration of 35%, raise the temperature to 40°C, react for 3h, and carry out vacuum distillation at 50°C and 0.8MPa for 5h to obtain 138g of 40% aziridine aqueous solution.

[0036]Preparation of refined aziridine: take 138g of 40% aziridine aqueous solution, add 61g of sodium hydroxide in a reaction kettle with a temperature of 5°C, start stirring to make the sodium hydroxide solution reach saturation, and continue to add 30g when it is not saturated Tablet alkali, until the reaction solution reaches saturation, stir for 2h, stand for 3h, the stand temperature is 5°C, after the stand, transfer the upper layer of aziridine to the rectification kettle, vent nitrogen, carry out rectification, the rect...

Embodiment 2

[0041] Preparation of crude 2-methyl aziridine: Accurately weigh 67g of isopropanolamine, add 120g of 98% concentrated sulfuric acid dropwise at room temperature, finish dropping after 4 hours, keep temperature at 70°C after dropping, keep hold for 3h, 90°C, 0.5 MPa for vacuum distillation, steamed for 3h, cooled to 30°C, added 205g sodium hydroxide aqueous solution with a mass concentration of 35%, heated up at 40°C, reacted for 3h, 50°C, 0.8MPa for 5h, and obtained a content of 48 % methyl aziridine aqueous solution 158g.

[0042] Preparation of refined aziridine: take 158g of 48% methyl aziridine aqueous solution, add 80g of sodium hydroxide in a reaction kettle with a temperature of 5°C, start stirring to make the sodium hydroxide solution reach saturation, and continue to Add 10g of caustic soda until the reaction solution is saturated, stir for 2h, let stand for 3h, let stand at a temperature of 5°C, transfer the upper layer of 2-methylaziridine to the rectification kett...

Embodiment 3

[0047] Preparation of crude aziridine: Accurately weigh 67g of monoethanolamine, add 108g of 98% concentrated hydrochloric acid dropwise at room temperature, and finish dropping after 5 hours. , lower the temperature to 20°C, add 236g of sodium hydroxide aqueous solution with a mass concentration of 35%, raise the temperature to 40°C, react for 2h, and carry out vacuum distillation at 50°C and 0.8MPa for 3h to obtain 118g of 45% aziridine aqueous solution.

[0048] Preparation of refined aziridine: take 118g of 45% aziridine aqueous solution, add 61g of sodium hydroxide in a reaction kettle with a temperature of 8°C, start stirring to make the sodium hydroxide solution reach saturation, and continue to add 30g of it when it is not saturated Tablet alkali, until the reaction solution reaches saturation, stir for 2h, stand for 3h, the stand temperature is 8°C, after the stand is finished, transfer the upper layer aziridine to the rectification kettle, vent nitrogen, carry out rec...

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Abstract

The invention provides a preparation method of refined aziridine, and belongs to the field of chemical engineering. The preparation method comprises the following steps: (1) adding an aziridine crude product and sodium hydroxide into a reaction kettle at 0-10 DEG C, enabling the sodium hydroxide to be saturated in a system, stirring and standing; (2) separating an upper layer aziridine-containing oil phase from a lower layer sodium hydroxide aqueous solution; and (3) rectifying the aziridine separated in the step (2). The content of the prepared refined aziridine is more than 99%, the water content is less than 0.02%, and the refined aziridine can be used for manufacturing dyes, pesticides and digital photographing laser printing photosensitive materials, can also be used as or used for manufacturing resin curing agents, cross-linking agents, coating modifiers, polymers and the like, and is an important fine chemical engineering intermediate. The invention provides a novel method for refining aziridine, the purity of the obtained aziridine monomer is high, the energy consumption is greatly reduced, the sodium hydroxide aqueous solution can be recycled, and the method is an energy-saving, environment-friendly and efficient aziridine purification method.

Description

technical field [0001] The invention belongs to the field of chemical industry, and in particular relates to a novel preparation method of refined aziridine. Background technique [0002] Aziridine is a three-membered ring compound with strong reactivity, which can react with compounds with various functional groups. The reactions mainly include substitution reaction, ring-opening reaction and copolymerization reaction. Reactive macromolecular compounds can be obtained by ring-opening polymerization or copolymerization, which are widely used in the paper industry, adhesive synthesis, textile industry, cosmetics industry and other fields. Aziridine monomers can also be used in the manufacture of dyes, pesticides, photosensitive materials for digital photography and laser printing, and aziridine crosslinking agents. At present, the synthetic methods of aziridine monomer mainly include sulfuric esterification method, 2-chloroethylamine method, dichloroethane method, ethylene o...

Claims

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Application Information

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IPC IPC(8): C07D203/08
CPCC07D203/08
Inventor 沈健陈永军谢彤仇雪松陆兴旺
Owner 上海健倬生物科技有限公司