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Continuous and stable production of highly etherified hexamethoxymethylmelamine preparation method

A technology of hexamethoxymethyl melamine and hexamethylolated melamine, which is applied in the field of preparation of hexamethoxymethyl melamine, can solve the problem of unstable quality of hexamethoxymethyl melamine, high content of free formaldehyde and long reaction time and other problems, to achieve the effect of long reaction residence time, low free formaldehyde content and short reaction time

Active Publication Date: 2021-01-12
JIANGSU CHANGNENG ENERGY SAVING NEW MATERIALS SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0012] The technical problem to be solved by the present invention is that the quality of hexamethoxymethylmelamine prepared in the prior art is not stable, the content of free formaldehyde is high, the water content is high, and the reaction time is long. It provides a continuous and stable production of high etherification The preparation method of hexamethoxymethylmelamine, the hexamethoxymethylmelamine prepared by the preparation method provided by the present invention has the advantages of stable quality, low free formaldehyde content, low moisture content and short reaction time

Method used

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  • Continuous and stable production of highly etherified hexamethoxymethylmelamine preparation method
  • Continuous and stable production of highly etherified hexamethoxymethylmelamine preparation method
  • Continuous and stable production of highly etherified hexamethoxymethylmelamine preparation method

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Experimental program
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Embodiment 1

[0037] (1) Polyformaldehyde and hydrolysis polymerize into a formaldehyde aqueous solution with a mass concentration of 30% and heat it up to 70°C for later use. Melamine powder and water are prepared into melamine slurry at a weight ratio of 1:1 and keep warm at 25°C for later use. Prepare good quality The sodium hydroxide solution with a concentration of 10% is pumped into the catalyst I tank for standby, and the mold temperature controller of the twin-screw extruder is preheated to 60°C. Methanol is pumped into the head tank to raise the temperature to 60°C for standby, and nitric acid is pumped into the catalyst II tank for standby. Continuously add melamine slurry, 30% formaldehyde solution and 10% sodium hydroxide into twin-screw extruder to carry out methylolation reaction to obtain material I, wherein the melamine slurry flow rate is 25.7Kg / h, 30% The flow rate of formaldehyde solution is 70Kg / h, the flow rate of 10% sodium hydroxide solution is 0.42Kg / h, the length-to...

Embodiment 2 to Embodiment 4

[0043] The experiment of embodiment 2 to embodiment 4 is carried out according to each step of embodiment 1, and only difference is that reaction parameter is different, specifically see table 2, the product quality detection data of the hexamethoxymethyl melamine of the continuous quality stability that prepares is as follows Table 5 shows.

[0044] The reaction parameter of table 2 embodiment 1 to embodiment 4

[0045]

[0046]

Embodiment 5 to Embodiment 8

[0048] The experiment of embodiment 5 to embodiment 8 is carried out according to each step of embodiment 1, and only difference is that reaction parameter is different, specifically see table 3, the product quality inspection data of the hexamethoxymethyl melamine of the continuous quality stability that prepares is as follows Table 5 shows.

[0049] The reaction parameter of table 3 embodiment 5 to embodiment 8

[0050]

[0051]

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Abstract

The invention relates to a preparation method for continuously and stably producing highly etherified hexamethoxymethyl melamine, and mainly solves the problems of unstable quality, high content of free formaldehyde, high moisture and long reaction time of hexamethoxymethyl melamine in the prior art. The method comprises the following steps: continuously adding melamine, formaldehyde and a catalyst I into a double-screw reactor for hydroxymethylation reaction to obtain a material I; continuously feeding the material I into a vacuum drying machine for drying, and grinding the material I to obtain hexamethylol melamine powder II; continuously conveying the material II, methanol and a catalyst II into an etherification reaction kettle for etherification reaction to obtain a material III; continuously introducing the material III into a neutralization kettle, adding a terminating agent, and terminating the etherification reaction to obtain a material IV; and continuously distilling and filtering the material IV to obtain the final product hexamethoxymethyl melamine. According to the technical scheme, a relatively good technical effect is achieved.

Description

technical field [0001] The invention relates to a preparation method for continuous and stable production of highly etherified hexamethoxymethylmelamine. Background technique [0002] Hexamethoxymethylmelamine resin, as the main cross-linking agent of coatings, is the most cost-effective and widely used. It is soluble in both water and organic solvents, which is conducive to the preparation of high-solid coatings and water-based coatings. It has the characteristics of high reactivity, good adhesion, good compatibility, hydrolysis resistance, high gloss, good storage stability, and excellent fluidity. It is not only used in the field of coatings such as automotive paint, coil material, iron printing, industrial paint, and wood paint. In addition, it can also be used in ink industry, paper industry, leather industry, etc. [0003] Hexamethoxymethylmelamine resin is used as the main adhesive of rubber, and it is used to compound with the loading body to form a methylene donor ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D251/64C08G12/42
CPCC07D251/64C08G12/427
Inventor 范勤勇陈玉赵俊飞李少杰朱益林
Owner JIANGSU CHANGNENG ENERGY SAVING NEW MATERIALS SCI & TECH
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