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Synthetic method of industrial additive N-ethyl phthalimide

A technology of ethyl phthalimide and phthalimide, which is applied in the field of synthesis of new industrial auxiliary agent N-ethyl phthalimide, can solve the problem of high price and production cost Problems such as remaining high and production costs unable to meet large-scale use

Inactive Publication Date: 2018-09-21
仪征市海帆化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The two substrates are expensive, and the production cost cannot satisfy the final product, which is used in large quantities as cheap industrial additives
The post-treatment process is complicated, there are many three wastes, and the production cost remains high

Method used

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  • Synthetic method of industrial additive N-ethyl phthalimide
  • Synthetic method of industrial additive N-ethyl phthalimide
  • Synthetic method of industrial additive N-ethyl phthalimide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] In a 500ml stainless steel magnetically stirred autoclave, add 100g (0.68mol) phthalimide, 20ml mass ratio of 2% acetonitrile solution of potassium phthalimide, 250ml acetonitrile and 5g benzyl peroxide Acyl, closed reactor. After the air in the kettle was replaced with nitrogen, stirring was started to raise the temperature.

[0033] When the temperature rose to 50°C, ethylene gas was introduced at this time. With the introduction of ethylene, the temperature in the kettle gradually increased. Regulate the feed rate of ethylene, and control the temperature in the kettle not to exceed 100°C. When the amount of feeding ethylene reached 35g, stop feeding ethylene. Incubate at 100°C for 3 hours. After the heat preservation is over, the gas in the kettle is replaced with nitrogen, and the liquid reaction solution is poured out. Transfer to a rotary evaporator.

[0034] Acetonitrile was distilled under normal pressure, and when 170ml of distillate was evaporated, the d...

Embodiment 2

[0036] In the stainless steel magnetic stirring autoclave of 500ml, add 100g (0.68mol) phthalimide, 20ml mass ratio is the acetonitrile solution of 2% potassium phthalimide, 250ml acetonitrile and 10g ditertiary peroxide Butyl, closed reactor. After the air in the kettle was replaced with nitrogen, stirring was started to raise the temperature.

[0037] When the temperature rose to 50°C, ethylene gas was introduced at this time. With the introduction of ethylene, the temperature in the kettle gradually increased. Regulate the feeding rate of ethylene, and control the temperature in the kettle not to exceed 85°C. When the amount of feeding ethylene reached 35g, stop feeding ethylene. Incubate at 85°C for 5 hours. After the heat preservation is over, the gas in the kettle is replaced with nitrogen, and the liquid reaction solution is poured out. Transfer to a rotary evaporator.

[0038] Acetonitrile was distilled under normal pressure, and when 170ml of distillate was evap...

Embodiment 3

[0040] In a 500ml stainless steel magnetically stirred autoclave, add 100g (0.68mol) phthalimide, 30ml mass ratio of 2% acetonitrile solution of potassium phthalimide, 250ml acetone and 8g ditertiary peroxide Butyl, closed reactor. After replacing the air in the kettle with nitrogen, stirring was started.

[0041]Ethylene gas is introduced at room temperature. With the introduction of ethylene, the temperature in the kettle gradually increased. Regulate the feeding rate of ethylene, and control the temperature in the kettle not to exceed 50°C. When the amount of feeding ethylene reached 35g, stop feeding ethylene. Incubate at 50°C for 5 hours. After the heat preservation is over, the gas in the kettle is replaced with nitrogen, and the liquid reaction solution is poured out. Transfer to a rotary evaporator.

[0042] Distill acetonitrile and acetone at atmospheric pressure, and stop distillation when 190ml of distillate is evaporated. Cool to 70°C, filter potassium phtha...

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Abstract

The invention discloses a synthetic method of industrial additive N-ethyl phthalimide. The synthetic method includes the steps: taking phthalimide and ethylene as main reaction substrates to perform free radical addition reaction under the condition of an initiator to obtain the N-ethyl phthalimide. The molar ratio of the phthalimide to the ethylene in a reaction system is 1:1-1:3, the initiator is an organic peroxide, the dosage of the organic peroxide initiator accounts for 5-10% of the weight of the phthalimide, reaction temperature ranges from 50 DEG C to 100 DEG C, and reaction time ranges from 3 hours to 5 hours. According to the method, the used phthalimide and the used ethylene are low in cost and easy to get, and the method has the advantages of mild reaction condition and low production cost.

Description

technical field [0001] The invention relates to a synthesis method of a novel industrial auxiliary agent N-ethylphthalimide. Background technique [0002] N-ethylphthalimide, the molecular structure is: [0003] [0004] N-ethylphthalimide, also known as N-ethylphthalimide, is a kind of N-substituted alkylphthalimide. Mainly used as industrial additives in textile, printing and dyeing, cosmetics, ink and other industrial fields. Domestic and foreign commodities are EPI. N-Ethylphthalimide (EPI) is a non-toxic and environmentally friendly industrial additive approved by EU REACH. Widely used in textile, printing and dyeing, cosmetics, ink and other industrial fields. As a carrier of disperse dyes, N-ethylphthalimide is used in the printing and dyeing industry. It has the advantages of being non-toxic, improving the production environment, and simplifying the dyeing process. Therefore, it is widely used in polyester, spandex, acrylic and cotton During fabric dyeing. I...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D209/48
CPCC07D209/48
Inventor 邹从伟戴久坤周芬沈永刚邹从欢
Owner 仪征市海帆化工有限公司
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