Continuous preparation method for preparing hexamethoxyl methyl melamine resin through continuous process

A technology of hexamethoxymethylmelamine and continuous method, which is applied in the field of continuous preparation of hexamethoxymethylmelamine resin by continuous method, can solve the problems of long production cycle, low degree of methyl etherification, high product viscosity, etc., and achieve operation Fewer personnel, no three wastes, high degree of automation

Inactive Publication Date: 2014-02-05
ZHANGJIAGANG SHUNCHANG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Domestic reports use inorganic bases (such as sodium hydroxide, sodium carbonate, etc.) as catalysts for methylolation and inorganic acids (such as hydrochloric acid, nitric acid, etc.) The

Method used

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  • Continuous preparation method for preparing hexamethoxyl methyl melamine resin through continuous process
  • Continuous preparation method for preparing hexamethoxyl methyl melamine resin through continuous process
  • Continuous preparation method for preparing hexamethoxyl methyl melamine resin through continuous process

Examples

Experimental program
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Effect test

Embodiment 1

[0030] 1) The configuration of melamine and methanol (or formalin, or aldol composite solution) slurry:

[0031] A component melamine slurry, put 335g melamine and 390g methanol into a 1 liter four-necked flask, beat at normal temperature, and set aside;

[0032] 2) Formalin solution configuration:

[0033] For component B formaldehyde solution, configure formaldehyde solution with a concentration of 45% (concentration can be between 25-65% according to needs). If the concentration is too low, you can use paraformaldehyde to depolymerize to prepare a formaldehyde solution with a suitable concentration for use;

[0034] 3) Hydroxymethylation reaction: Put A and B components into the methylolation reactor according to A:B=1:1.5 (weight ratio), add a certain amount of triethylamine (or other amines compound), control the reaction temperature at 45-85°C, pH=7.5-10.0, and the reaction time for 10-90 minutes to obtain low methylolated melamine, continue the methylolation reaction, ...

Embodiment 2

[0044] 1) The configuration of melamine and methanol (or formalin, or aldol composite solution) slurry:

[0045] A component melamine slurry, put 33.5kg melamine and 450kg methanol into a 1000-liter reactor, beat at normal temperature, and set aside;

[0046] 2) Formalin solution configuration:

[0047] For component B formaldehyde solution, configure formaldehyde solution with a concentration of 45% (concentration can be between 25-65% according to needs). If the concentration is too low, you can use paraformaldehyde to depolymerize to prepare a formaldehyde solution with a suitable concentration for use;

[0048] 3) Hydroxymethylation reaction: Put A and B components into the continuous methylolation reactor according to A:B=1:1.5 (weight ratio), add a certain amount of triethylamine (or other amines compound), control the reaction temperature at 45-85°C, pH value 7.5-10.0, and reaction time 10-90 minutes to obtain low methylolated melamine, and pump low methylolated melami...

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Abstract

The invention discloses a preparation method for preparing hexamethoxyl methyl melamine resin through a continuous process, and belongs to the field of organic synthesis. The preparation method comprises the following steps: 1) carrying out continuous reaction on melamine and a formaldehyde water solution by taking inorganic base as a catalyst to obtain hexahydroxy methyl melamine; 2) carrying out continuous vacuum drying on the hexahydroxy methyl melamine until the water content is less than 1%, and smashing; 3) regulating the pH of the hexahydroxy methyl melamine and methanol by use of an organic acid, and carrying out a continuous etherification reaction; 4) continuously distilling a product obtained from the etherification reaction, and removing impurities to obtain the hexamethoxyl methyl melamine resin (II). According to the process, the organic base is adopted for replacing a conventional inorganic base as a catalyst in hydroxymethylation, so that production is more stable, and melamine is used; the organic acid is used as a catalyst in esterification, which is beneficial to oxidation and neutralization in the later period of reaction. An oxidizing agent is adopted to terminate the esterification, so that the product is free from generation of solid salt and free from precipitation of solid after low-boiling-point substances are recovered, thus omitting solid and liquid separation.

Description

technical field [0001] The invention belongs to the field of organic synthesis, and in particular relates to a continuous preparation method for preparing hexamethoxymethylmelamine resin by a continuous method. Background technique [0002] Hexamethoxymethyl melamine resin is a kind of melamine resin (or melamine formaldehyde resin, or amino resin). Due to the deep etherification after methylolation, the product has good cross-linking performance and can be Widely used in water-based system coatings, metal coatings, textile coatings, etc. [0003] Domestic reports use inorganic bases (such as sodium hydroxide, sodium carbonate, etc.) as catalysts for methylolation and inorganic acids (such as hydrochloric acid, nitric acid, etc.) The production cycle of the product is long, and all of them adopt batch production technology. The batch production has the disadvantages of low degree of methyl etherification and high product viscosity. Contents of the invention [0004] The ...

Claims

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Application Information

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IPC IPC(8): C07D251/64C08G12/42
CPCC07D251/64
Inventor 蒋建平顾丰平
Owner ZHANGJIAGANG SHUNCHANG CHEM
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