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ChemicalBook CAS DataBase List Tris(dimethylaminomethyl)phenol
90-72-2

Tris(dimethylaminomethyl)phenol synthesis

4synthesis methods
-

Yield:-

Reaction Conditions:

Stage #1: formaldehyd;dimethyl amine in water at 60; under 3000.3 Torr; for 5 h;Large scale;
Stage #2: phenol in water at 90; for 3.5 h;Large scale;Temperature;

Steps:

1-3 This embodiment includes the following steps:

(1) Weigh 3600kg of dimethylamine (concentration 40wt%) into a 6m3 batch stirring reactor, the stirring speed is controlled at 40r/min, then weigh 1800kg of formaldehyde (concentration 40wt%), and use a metering pump to control it evenly within 2.5 hours Add the dimethylamine aqueous solution to the reaction. After the addition is completed, the temperature is raised to 60°C under a pressure of 0.4Mpa (with a certain pressure, which can effectively avoid the gasification and material loss of formaldehyde and dimethylamine caused by the increase in reactivity), React for 2.5 hours to obtain a solution system;(2) Weigh 180kg of phenol and add it to the solution system obtained in step (1) uniformly within 1.5 hours by using a metering pump, then heat to 90°C, react for 2h, stand for layering, separate oil and water, the lower layer is the water phase, and enter Water phase storage tank, the upper layer for the target product enters the oil-water separator for oil-water separation again, the separated organic phase enters the product storage tank, and the water phase enters the water phase storage tank;(3) The water phase obtained in step (2) is heated to the bubble point temperature and enters the first rectification tower. An aqueous solution of dimethylamine (concentration 40wt%) is extracted from the top of the tower. The temperature is controlled at 10°C and the pressure is 0.11Mpa. Return to step (1) As a raw material, the temperature of the bottom of the tower is 90 and the pressure is 0.13Mpa. The aqueous solution discharged from the bottom of the tower enters the second rectification tower, and the aqueous solution produced at the top of the second rectification tower is sent to the biochemical unit. The top temperature is 35 and the pressure is 0.11. Mpa, the material discharged from the tower is sent to step (2) as raw material.

References:

CN111072501,2020,A Location in patent:Paragraph 0027-0049

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