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Method for synthesizing 2, 4, 6-tri(dimethylamino methyl) phenol

A technology of dimethylaminomethyl and phenol is applied in the field of chemistry to achieve the effects of increasing production cost, reducing energy consumption and high transportation cost

Inactive Publication Date: 2012-10-24
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In the new synthesis method, the in-situ depolymerization solution of paraformaldehyde is used instead of the aqueous formaldehyde solution to participate in the reaction. The use of paraformaldehyde not only solves the problems of the transportation and storage of the aqueous formaldehyde solution and the introduction of a large amount of water in the raw materials, but also in The heat released during the depolymerization process will promote the reaction, and reduce the amount of waste water generated after the reaction, simplify the subsequent treatment process, reduce energy consumption, and benefit environmental protection

Method used

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  • Method for synthesizing 2, 4, 6-tri(dimethylamino methyl) phenol
  • Method for synthesizing 2, 4, 6-tri(dimethylamino methyl) phenol
  • Method for synthesizing 2, 4, 6-tri(dimethylamino methyl) phenol

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Effect test

Embodiment 1

[0030] In a 500ml four-neck flask equipped with a stirring, reflux device, and a thermometer, add 28.2g of phenol and 135g of dimethylamine aqueous solution, and stir at room temperature for 15-30min to make it evenly mixed; then at a temperature of 20-50°C, Add 28.4g of paraformaldehyde several times within 1 hour; react the mixture at 70-80°C for 2-3 hours; then carry out oil-water separation and vacuum distillation to remove water from the product, and collect the product. The obtained product is a light yellow transparent liquid with a viscosity of 150-250mpa·s and an amine value of 600-630mgKOH / g. Its infrared spectrum is as attached figure 1 As shown, the H NMR spectrum is shown in the attached figure 2 shown. The amount of waste water produced after the reaction was about 112g. And as an accelerator, the effect is obvious.

Embodiment 2

[0034] Add 355kg of phenol and 1544kg of dimethylamine aqueous solution into the reaction kettle, and mix them uniformly at room temperature; then add 358kg of paraformaldehyde powder into the reaction kettle in fractions within 1 hour at a temperature of 20-50°C , make the mixed solution react at 70-80°C for 2-3 hours; then carry out oil-water separation and vacuum distillation to remove the water in the product, and collect the product. The obtained product is a light yellow transparent liquid with a viscosity of 150-250mpa·s and an amine value of 600-630mgKOH / g. The amount of waste water produced after the reaction is about 1300kg.

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Abstract

The invention relates to a novel method for synthesizing epoxy resin accelerator (curing agent)-2, 4, 6-tri(dimethylamino methyl) phenol. 2, 4, 6-tri(dimethylamino methyl) phenol is prepared from in-situ depolymerization solution of paraformaldehyde, phenol and dimethylamine aqueous solution through Mannich condensation reaction. The method is characterized in that the phenol and the dimethylamine aqueous solution are uniformly mixed at the temperature between 0-70 DEG C, and quantitative paraformaldehyde is added within 0.5-1 hour in batches, so the mixture is enabled to react for 1-4 hours at the temperature between 30-100 DEG C; and after discharging, oil-water separation and reduced-pressure distillation, 2, 4, 6-tri(dimethylamino methyl) phenol can be obtained. The method adopts the in-situ depolymerization solution of paraformaldehyde to substitute formaldehyde aqueous solution to react, so the problems of inconvenient formaldehyde aqueous solution transportation and storage, a great deal of product wastewater after the reaction, larger energy consumption and the like in the traditional synthesizing technology are effectively solved.

Description

Technical field: [0001] The invention relates to a method for synthesizing 2,4,6-tris(dimethylaminomethyl)phenol, in particular to synthesizing 2,4,6-tris(dimethylaminomethyl)by in-situ depolymerization reaction of paraformaldehyde ) A novel method for phenol, which belongs to the field of chemistry. Background technique: [0002] Epoxy resins must be added with a curing agent when used, and an excellent curing agent can make the epoxy resin cured product have excellent performance. Through the curing reaction, the epoxy resin can form a three-dimensional network structure and become an epoxy resin material with real use value. [0003] The curing agent determines the excellent performance of the epoxy resin to a certain extent. The mechanism of the reaction between the epoxy resin and the curing agent is to open the epoxy group through the active hydrogen contained in the curing agent, so that the epoxy resin undergoes a crosslinking reaction and then solidify. Commonly ...

Claims

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Application Information

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IPC IPC(8): C07C215/50C07C213/02
Inventor 徐世爱刘媛彭青海
Owner EAST CHINA UNIV OF SCI & TECH
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