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Prepn process of 4,4'-methylene-bis(2,6-diethyl aniline) (MDEA)

A technology of diethylaniline and methylene, which is applied in the field of polymer material synthesis, can solve problems such as no relevant reports, and achieve the effects of low preparation cost, high purity and yield, and easy availability of raw materials

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 MDEA, according to the literature search, there is no relevant report

Method used

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

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] 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 DEA (2,6-diethylaniline) weighed. Then, the weighed 133g hydrochloric acid (28%) was added in the flask with a separatory funnel, and the feed liquid was heated to 50°C. Add the weighed 52g formaldehyde solution (30%) 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 80°C for another 2 hours. After the reaction is completed, 30% NaOH solution is added to neutralize the feed liquid until the feed liquid pH=7.5-8. 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 MDEA after removing the water layer. The crude MDEA product is decolorized by activated carbon, dehydrated under reduced pressure, crystallized and granul...

Embodiment 2

[0028] 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 DEA (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 52g 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 MDEA after removing the water layer. The crude product of MDEA is decolorized by ethanol recrystallization, filtered, dried and granulated to obtai...

Embodiment 3

[0030] 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 DEA (2,6-diethylaniline) weighed. Then, add weighed 150g hydrochloric acid (33%) in the flask with a separatory funnel, and heat the feed liquid to 60°C. Add the weighed 65g 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 MDEA after removing the water layer. The crude MDEA is decolorized through ultrafiltration membrane filtration, dehydrated under reduced pressure, crystallized, ...

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Abstract

The preparation process of 4, 4'-methylene-bis-(2, 6-diethyl aniline) (MDEA) belongs to the field of polymer synthesis technology. Under the protection of inert gas, material 2, 6-diethyl aniline is dissolved in water and hydrochloric acid in certain amount is added to produce 2, 6-diethyl aniline hydrochloride. Then, water solution of formaldehyde in stoichiometric amount is dropped while heating to produce condensation; and through maintaining the temperature for finishing the reaction and neutralization with alkali, coarse MDEA product is separated. Through further decolorizing, dewatering, crystallizing and pelletizing, MDEA product is obtained. The preparation process is simple and has mild reaction condition, low production cost and high yield, and MDEA has less 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-(2,6-diethylaniline) [MDEA] 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 as: vario...

Claims

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Application Information

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IPC IPC(8): C07C211/50
Inventor 陆锦贤
Owner 陆锦贤
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