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, accord

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
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Effect test

Example Embodiment

[0018] Example 1

[0019] Put 400g of water (tap water or distilled water) into a 1000ml four-necked flask with stirring and nitrogen protection device, turn on the stirring, and slowly add the weighed 150g DEA (2,6-diethylaniline). Then, the weighed 133g of hydrochloric acid (28%) was added into the flask with a separatory funnel, and the feed solution was heated to 50°C. Then 52 g of formaldehyde solution (30%) weighed was added dropwise to the flask to carry out the condensation reaction, the drop was completed in about 60 minutes, and then the temperature was kept for 1 hour. Then heat to 80°C and keep for 2 hours. After the reaction is over, 30% NaOH solution is added to neutralize the material liquid until the pH of the material liquid is 7.5-8. Stand still for 30 minutes, divide the water layer with a separatory funnel, and wash the material twice with an appropriate amount of hot water, and then get the crude MDEA product after pumping off the water layer. The crude MDEA p...

Example Embodiment

[0027] Example 2

[0028] Put 400g of water (tap water or distilled water) into a 1000ml four-necked flask with stirring and nitrogen protection device, turn on the stirring, and slowly add the weighed 150g DEA (2,6-diethylaniline). Then, add 155 g of hydrochloric acid (28%) weighed into the flask with a separatory funnel, and heat the feed solution to 60°C. Then weighed 52 g of formaldehyde solution (37%) was added dropwise to the flask to carry out the condensation reaction, the drop was completed in about 60 minutes, and then the temperature was kept for 1 hour. Then heat to 90°C and keep for 2 hours. After the reaction is over, add 30% Na 2 CO 3 The solution neutralizes the feed liquid to the pH of the feed liquid = 8-9. Stand still for 30 minutes, divide the water layer with a separatory funnel, and wash the material twice with an appropriate amount of hot water, and then get the crude MDEA product after pumping off the water layer. The crude MDEA product is decolorized by et...

Example Embodiment

[0029] Example 3

[0030] Put 400g of water (tap water or distilled water) into a 1000ml four-necked flask with stirring and nitrogen protection device, turn on the stirring, and slowly add the weighed 150g DEA (2,6-diethylaniline). Then, the weighed 150g hydrochloric acid (33%) was added into the flask with a separatory funnel, and the feed solution was heated to 60°C. Then the weighed 65g formaldehyde solution (35%) was added dropwise to the flask for condensation reaction, the drop was completed in about 60 minutes, and then the temperature was kept for 1 hour. Then heat to 90°C and keep for 2 hours. After the reaction is over, 30% NaOH solution is added to neutralize the material liquid until the pH of the material liquid is 9-10. Stand still for 30 minutes, divide the water layer with a separatory funnel, and wash the material twice with an appropriate amount of hot water, and then get the crude MDEA product after pumping off the water layer. The crude MDEA product is filtere...

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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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