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Prepn process of 4,4'-methylene-bis(3-chloro-2,6-diethyl aniline) (MCDEA)

A technology of diethylaniline and diethylbenzene, applied in the field of polymer material synthesis, can solve problems such as no preparation reports, and achieve the effects of uncomplicated process, low price, high purity and yield

Inactive Publication Date: 2005-12-14
陆锦贤
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] At present, the preparation method of MCDEA, there is no report on the preparation of this substance in China

Method used

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  • Prepn process of 4,4'-methylene-bis(3-chloro-2,6-diethyl aniline) (MCDEA)
  • Prepn process of 4,4'-methylene-bis(3-chloro-2,6-diethyl aniline) (MCDEA)
  • Prepn process of 4,4'-methylene-bis(3-chloro-2,6-diethyl aniline) (MCDEA)

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Put 400g of water (tap water or distilled water) in a 1000ml four-neck flask with stirring and nitrogen protection device, start stirring, and slowly add 150g of CDEA (3-chloro-2,6-diethylaniline) weighed. Then, add 120g of hydrochloric acid with a weighed concentration of 31% into the flask with a separatory funnel, heat the feed liquid to 50°C, then drop 50g of formaldehyde solution with a weighed concentration of 30% into the flask for condensation Reaction, drop in about 60 minutes, then keep warm for 1 hour, then warm to 80°C and keep warm for 2 hours. After the reaction is over, add 30% NaOH solution to neutralize the feed liquid until the feed liquid pH=7.5-8, and stand still for 30 minutes , Use a separatory funnel to separate the water layer, and wash the material twice with an appropriate amount of hot water, and get the crude MCDEA after removing the water layer. The crude MCDEA is decolorized by activated carbon, dehydrated under reduced pressure, crystalliz...

Embodiment 2

[0027] Put 400g of water (tap water or distilled water) in a 1000ml four-neck flask with stirring and nitrogen protection device, start stirring, and slowly add 150g of CDEA (3-chloro-2,6-diethylaniline) weighed. Then, the weighed 155g hydrochloric acid (28%) was added in the flask with a separatory funnel, and the feed liquid was heated to 60°C. Add the weighed 45g formaldehyde solution (37%) dropwise in the flask to carry out the condensation reaction, drop it in about 60 minutes, and then keep warm for 1 hour. Reheat to 90°C for another 2 hours. After the reaction is over, add 30% Na 2 CO 3 The solution neutralizes the feed liquid until the pH of the feed liquid is 8-9. Stand still for 30 minutes, use a separatory funnel to separate the water layer, and wash the material twice with an appropriate amount of hot water, and get the crude MCDEA after removing the water layer. The crude MCDEA is decolorized by ethanol recrystallization, filtered, dried, and granulated to obt...

Embodiment 3

[0029] Put 400g of water (tap water or distilled water) in a 1000ml four-neck flask with stirring and nitrogen protection device, start stirring, and slowly add 150g of CDEA (3-chloro-2,6-diethylaniline) weighed. Then, the weighed 140g hydrochloric acid (33%) was added in the flask with a separatory funnel, and the feed liquid was heated to 60°C. Add the weighed 63g formaldehyde solution (35%) dropwise in the flask to carry out the condensation reaction, drop it in about 60 minutes, and then keep warm for 1 hour. Reheat to 90°C for another 2 hours. After the reaction is completed, 30% NaOH solution is added to neutralize the feed liquid until the pH of the feed liquid is 9-10. Stand still for 30 minutes, use a separatory funnel to separate the water layer, and wash the material twice with an appropriate amount of hot water, and get the crude MCDEA after removing the water layer. The crude MCDEA is decolorized by ultrafiltration, dehydrated under reduced pressure, crystallize...

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Abstract

The preparation process of 4, 4'-methylene-bis-(3-chloro-2, 6-diehtyl aniline) (MCDEA) belongs to the field of polymer synthesis technology. Under the protection of inert gas, material 3-chloro-2, 6-diehtyl aniline is reacted with hydrochloric acid in water solution to produce 3-chloro-2, 6-diehtyl aniline hydrochloride. Then, water solution of formaldehyde is dropped while heating to produce condensation; and through maintaining the temperature for finishing the reaction and neutralization with alkali, coarse MCDEA product is separated. Through further decolorizing, dewatering, crystallizing and pelletizing, MCDEA product is obtained. The preparation process is simple and has mild reaction condition, low production cost and high yield, and MCDEA has micro toxicity and may be used to replace MOCA as chain expander for PU material.

Description

technical field [0001] The invention belongs to the field of polymer material synthesis, and relates to a preparation method of chain extender 4,4'-methylene-bis-(3-chloro-2,6-diethylaniline) [MCDEA] for polyurethane synthesis. Background technique [0002] The research and development of polyurethane (referred to as PU) materials has a history of more than 60 years. In the past 40 years, all kinds of PU materials have developed rapidly, and the output has increased by more than 2,000 times. In the past 20 years, the output of PU materials in my country has also increased by more than 20 times. With the continuous expansion of the application of PU materials, the number of its products has jumped to the top of the world's six major synthetic materials, and the global output is about 10 million tons. [0003] Due to its excellent performance, PU materials are widely used in various fields of the national economy and in all aspects of people's basic necessities of life. Such...

Claims

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Application Information

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IPC IPC(8): C07C211/52
Inventor 陆锦贤
Owner 陆锦贤
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