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A kind of production method of 2,4,6-tris(dimethylaminomethyl)phenol

A production method of dimethylaminomethyl, which is applied in the field of epoxy resin curing catalyst preparation, can solve the problems of increasing the difficulty of wastewater treatment and low yield, reduce the amount of amine substances and wastewater, and improve Yield and cost reduction effect

Active Publication Date: 2021-06-11
岳阳中展科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The synthesis process is to add phenol and dimethylamine aqueous solution first, after mixing evenly, add formaldehyde aqueous solution dropwise, after the dropwise addition, heat up to 90-95°C for reaction, after the reaction is completed, oil and water are separated, the organic phase is concentrated under reduced pressure, and distilled. Obtain 2,4,6-tris(dimethylaminomethyl)phenol, the yield is less than 85%
Through research, it has been found that formaldehyde will be dropped into the mixed solution of dimethylamine and phenol, and formaldehyde will participate in side reactions outside the main reaction, as shown in formula II, by-products such as hydroxybenzyl alcohol and o-hydroxybenzyl alcohol will be produced. By-products and incompletely reacted dimethylamine are enriched in strong alkaline wastewater, which increases the difficulty of wastewater treatment
Simultaneously, because the generation of side reaction and the existence of incompletely reacted mono-substituted and double-substituted intermediates make the yield of reaction lower, lower than 85% all the time

Method used

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  • A kind of production method of 2,4,6-tris(dimethylaminomethyl)phenol
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  • A kind of production method of 2,4,6-tris(dimethylaminomethyl)phenol

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Embodiment 1

[0028] This embodiment includes the following steps:

[0029] (1) Weigh 1800kg dimethylamine (concentration 40wt%) and add 6m 3 The intermittent stirring reactor, the stirring speed is controlled at 40r / min, then weighed 1000kg of formaldehyde (concentration 40wt%), controlled by a metering pump and added to the dimethylamine aqueous solution to react within 1.5 hours, and the temperature was raised to 60°C after the feeding was completed. Under the 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 hours to obtain a solution system;

[0030] (2) Weigh 120kg of phenol, control it with a metering pump and add it into the solution system obtained in step (1) within 1.5 hours, then raise the temperature to 90°C, react for 3 hours, let stand to separate layers, separate oil and water, the lower layer is the water phase, enter Water phase st...

Embodiment 2

[0033] This embodiment includes the following steps:

[0034] (1) Weigh 3600kg dimethylamine (concentration 40wt%) and add 6m 3 The intermittent stirring reactor, the stirring speed is controlled at 40r / min, then weighed 1800kg of formaldehyde (concentration 40wt%), controlled by a metering pump and added to the dimethylamine aqueous solution to react within 2.5 hours, and the temperature was raised to 60°C after the feeding was completed. Under the 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;

[0035] (2) Weigh 180kg of phenol, and use a metering pump to control it and add it into the solution system obtained in step (1) within 1.5 hours, then raise the temperature to 90°C, react for 2 hours, leave to separate layers, separate oil and water, the lower layer is the water phase, enter Water phas...

Embodiment 3

[0038] This embodiment includes the following steps:

[0039] (1) Weigh 3600kg dimethylamine (concentration 40wt%) and add 6m 3 The intermittent stirring reactor, the stirring speed is controlled at 40r / min, then weighed 1600kg of formaldehyde (concentration 40wt%), controlled by a metering pump and added to the dimethylamine aqueous solution to react within 2.5 hours, and the temperature was raised to 50°C after the feeding was completed. Under the 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 3 hours to obtain a solution system;

[0040] (2) Weigh 160kg of phenol, and use a metering pump to control it and add it into the solution system obtained in step (1) within 1.5 hours, then raise the temperature to 90°C, react for 3 hours, leave to separate layers, separate oil and water, the lower layer is the water phase, enter Water phase ...

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Abstract

A method for producing 2,4,6-tris(dimethylaminomethyl)phenol. The method of the present invention comprises the following steps: (1) adding formaldehyde to dimethylamine, then raising the temperature to 50-60°C, and reacting for 1-3 hours to obtain a solution system; (2) adding phenol to the solution system obtained in step (1) , then raise the temperature to 80-90°C, react for 1.5-4 hours, stand to separate layers, and separate oil and water. The upper layer is the target product, and the lower layer is the water phase; (3) The water phase obtained in step (2) is sent to the double-column rectification, The aqueous solution of dimethylamine is extracted from the top of the first rectification tower, and returned to step (1) as a raw material, the aqueous solution discharged from the bottom of the first rectification tower enters the second rectification tower, and the aqueous solution is extracted from the top of the second rectification tower It is sent to the biochemical device, and the material discharged from the bottom of the second rectification tower is sent to step (2) as a raw material. The production method of the invention has high yield, less by-products and less sewage.

Description

technical field [0001] The invention relates to the field of preparation of epoxy resin curing catalysts, in particular to a production method of 2,4,6-tris(dimethylaminomethyl)phenol. Background technique [0002] 2,4,6-tris(dimethylaminomethyl)phenol (DMP-30) is a curing catalyst for thermosetting epoxy resin, which can greatly increase the reaction speed of curing agent and epoxy resin and reduce the curing temperature without affecting the adhesive physical and chemical properties. Compared with other curing agents, it has good catalytic effect and complete reaction, and is suitable for low-temperature, high-temperature-resistant and low-molecular-weight rubber-modified epoxy adhesives and adhesives for some special purposes and special processes. Especially in recent years, with the development of epoxy resin and adhesive application, 2,4,6-tris(dimethylaminomethyl)phenol has been more widely used. [0003] [0004] At present, the synthesis of 2,4,6-tris(dimethyla...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C213/02C07C213/10C07C215/50
CPCC07C213/00C07C213/02C07C213/10C07C215/50C07C215/08
Inventor 孟勇余志良刘慧森
Owner 岳阳中展科技有限公司
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