Preparation method of bis(2-dimethyl aminoethyl) ether

A technology of dimethylaminoethyl and dimethylaminoethoxyethanol, which is applied in the field of chemical synthesis, can solve the problems of complex post-processing, cumbersome process, and low total yield, and achieve easy post-processing, easy-to-obtain raw materials, The effect of high total yield

Active Publication Date: 2013-12-18
GOLDENKEYS HIGH TECH MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has long steps, low efficiency and complex post-processing
[0006] Method 3: Domestic journals reported that the catalyst bis(dimethylaminoethyl)ether was synthesized with ethylene glycol and dimethylamine as raw materials. The reaction used a fixed-bed reactor, and the selectivity was low, with the highest selectivity being only 27.5%. The overall yield is low, and the generated dimethylaminoethoxyethanol needs to be separated, the process is cumbersome, and it is not suitable for large-scale industrial production

Method used

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  • Preparation method of bis(2-dimethyl aminoethyl) ether

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Comparison scheme
Effect test

Embodiment 1

[0021] (1) First add 133g (1mol) of dimethylaminoethoxyethanol to a 1L autoclave, then add 70g of water, then add 7g of Cu-Al / diatomite catalyst, and then blow nitrogen into the autoclave The air was replaced, and then 85g (5mol) of anhydrous liquid ammonia and 0.3Mpa hydrogen were introduced, and then the temperature was raised to 180°C, and the reaction was carried out at a reaction pressure of 10Mpa for 9 hours, and high-speed stirring was always maintained during the above reaction process; After completion, the temperature in the autoclave is lowered to normal temperature, the pressure is vented to normal pressure, then the material is discharged, the Cu-Al / diatomite catalyst is filtered, and the filtrate is rectified to obtain dimethylaminoethoxyethyl alcohol with a purity of 98.4%. Amine 95g;

[0022] (2), then put 66g (0.5mol) of dimethylaminoethoxyethylamine obtained in the previous step of rectification into the autoclave, then add 0.7g of Pd / C palladium carbon catal...

Embodiment 2

[0027] (1) First add 266g (2mol) of dimethylaminoethoxyethanol to a 1L autoclave, then add 150g of water, then add 27g of Cu-Al / diatomaceous earth catalyst, and then blow nitrogen into the autoclave Then, 180g (10.58mol) of anhydrous liquid ammonia and 0.5Mpa hydrogen gas were introduced, and then the temperature was raised to 160°C, and the reaction was carried out at a reaction pressure of 15Mpa for 5 hours, and high-speed stirring was always maintained during the above reaction process; After the reaction is completed, the temperature in the autoclave is lowered to normal temperature, the pressure is vented to normal pressure, then the material is discharged, the Cu-Al / diatomite catalyst is filtered, and the filtrate is rectified to obtain dimethylaminoethoxy with a purity of 98.5%. Ethylamine 195g;

[0028] (2), then put 132g (1mol) of dimethylaminoethoxyethylamine obtained in the previous step of rectification into the autoclave, then add 1g of Pd / C palladium carbon catal...

Embodiment 3

[0033](1) First add 266g (2mol) of dimethylaminoethoxyethanol to a 1L autoclave, then add 250g of water, then add 40g of Cu-Al / diatomaceous earth catalyst, and then blow nitrogen into the autoclave Then, 200g (11.76mol) of anhydrous liquid ammonia and 0.8Mpa hydrogen were introduced, and then the temperature was raised to 170°C, and the reaction was carried out at a reaction pressure of 8Mpa for 12 hours, and high-speed stirring was maintained throughout the above reaction process; After the reaction is completed, the temperature in the autoclave is lowered to normal temperature, the pressure is vented to normal pressure, then the material is discharged, the Cu-Al / diatomite catalyst is filtered, and the filtrate is rectified to obtain dimethylaminoethoxy with a purity of 98.6%. Ethylamine 199g;

[0034] (2), then put 132g (1mol) of dimethylaminoethoxyethylamine obtained in the previous step of rectification into the autoclave, then add 1.3g of Pd / C palladium carbon catalyst, a...

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Abstract

The invention discloses a preparation method of bis(2-dimethyl aminoethyl) ether. The preparation method comprises the following steps: adding dimethyaminoethoxyethanol, water and a Cu-Al / diatomite catalyst into a high-pressure reaction kettle, introducing nitrogen to perform replacement, introducing anhydrous liquid ammonia and hydrogen, heating to 100-250 DEG C, reacting for 3-15 hours under the pressure of 5-15 Mpa and keeping stirring; cooling and emptying to normal pressure after the reaction is finished, discharging, filtering the catalyst and rectifying filtrate; adding rectified dimethyaminoethoxyethanol, adding a Pd / C palladium carbon catalyst, introducing nitrogen to perform replacement, then introducing hydrogen to maintain the pressure to be 0.5-5 Mpa, heating to 50-60 DEG C, adding formaldehyde, heating to 60-150 DEG C, reacting for 3-10 hours under the pressure of 0.5-5 Mpa, introducing hydrogen and keeping stirring; cooling and emptying to normal pressure after the reaction is finished, discharging, filtering the catalyst and rectifying the filtrate to obtain the bis(2-dimethylaminoethyl) ether. The preparation method has the advantages of simple process and high yield.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, in particular to a preparation method of bis(2-dimethylaminoethyl) ether. Background technique [0002] Bis(2-dimethylaminoethyl) ether is a colorless transparent liquid. Soluble in water, easily soluble in alcohol, benzene, etc. As a high-efficiency tertiary amine catalyst, it is suitable for the production of almost all foam products, mainly for the production of flexible foam products, especially for high resilience products and RIM products. It is characterized by high catalytic activity, stable foaming, large tolerance to tin, and easy adjustment of formula. The physical and chemical properties of products produced with it are superior to other products such as rebound rate and elongation. [0003] In the prior art, the synthetic method of two (2-dimethylaminoethyl) ethers mainly contains following several kinds: [0004] Method 1: U.S. Patent No. 417721, using sodium 2-dimethylaminoetha...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C217/08C07C213/00
Inventor 陈松林黄达其
Owner GOLDENKEYS HIGH TECH MATERIALS CO LTD
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