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Preparation method of methylated melamine-formaldehyde resin

A technology for methyl-etherified melamine and etherified melamine, which is applied in the field of preparation of methyl-etherified melamine formaldehyde resin, can solve the problems of product quality difference, complicated process, inconvenient operation, etc., and achieves less free formaldehyde content and a degree of etherification. High and reduce the effect of process safety hidden danger risk

Active Publication Date: 2021-06-11
SHANDONG YANGGU HUATAI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The invention patent with application number 2020110369056 discloses a preparation method of methyl etherified melamine formaldehyde resin, which adopts the reaction kettle-type batch reaction preparation method. This batch method preparation method has product quality differences between batches problems, while the process is cumbersome and inconvenient to operate

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] A kind of preparation method of methylated melamine formaldehyde resin comprises the following steps:

[0022] Step 1: Quantitatively add formaldehyde, melamine and liquid caustic soda to the pipeline and transport at a constant speed. During the transportation process, the temperature is raised to 60-70°C, and the heat preservation reaction is carried out for 10-12 minutes; in the raw materials, the molar ratio of formaldehyde to melamine is 6.9-7.1: 1. PH control 8~9;

[0023] Step 2: After the heat preservation reaction is completed, quantitatively add methanol to the pipeline flowing at a constant speed, add hydrochloric acid after temperature control to adjust PH=3-4, keep heat for 5-7 minutes, and then add liquid caustic soda quantitatively to adjust PH=8-9; The methanol, melamine and methanol added in the molar ratio is 1:15~17; then the reaction system enters the thin film evaporator for negative pressure distillation to 65~70°C;

[0024] Step 3: Add the rough ...

Embodiment 2

[0026] A kind of preparation method of methylated melamine formaldehyde resin comprises the following steps:

[0027] Step 1: Quantitatively add formaldehyde, melamine and liquid caustic soda to the pipeline and transport it at a constant speed. During the process of transportation, the temperature is raised to 65°C. During the heating process, the circulating hot water heating system is used to heat the reaction system, and the reaction is kept for 11 minutes; among the raw materials, formaldehyde The molar ratio with melamine is 7.0:1, and the pH is controlled at 8.5;

[0028] Step 2: After the heat preservation reaction is completed, quantitatively add methanol to the pipeline flowing at a constant speed, and after temperature control, add hydrochloric acid to adjust the pH=3.5. During the temperature control process, use the warm water heating system and the circulating water cooling system to control the temperature of the reaction system; heat preservation reaction 6min ...

Embodiment 3

[0032] A preparation method of methyl etherified melamine formaldehyde resin, the steps are as follows:

[0033] Step 1: Feed 100g of melamine into the pipeline at a feed rate of 100g / h and 450g of formaldehyde at a feed rate of 450g / h, and at the same time feed liquid alkali quantitatively into the feed port to adjust the pH to 8-9, and immerse the pipeline at 70°C Heating and heat preservation reaction in hot water;

[0034] Step 2: After reacting for 11 minutes, quantitatively mix 406g of methanol with the reaction system, immerse the pipeline in water at 40°C for temperature control, add hydrochloric acid quantitatively to adjust PH = 3-4, and keep warm for 6 minutes, add liquid caustic soda quantitatively to adjust PH = 8~9; enter the evaporator at a constant speed for negative pressure distillation, and control the temperature of the semi-product after distillation to 70°C;

[0035] Step 3: Quantitatively mix the semi-product and 152g of methanol, immerse the pipeline i...

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Abstract

The invention discloses a preparation method of methylated melamine-formaldehyde resin , relates to the technical field of fine chemical engineering, and in particular relates to a preparation method of methylated melamine-formaldehyde resin. The method comprises the steps of 1, adding formaldehyde, melamine and caustic soda liquid into a pipeline, heating to 60-70 DEG C, and carrying out heat preservation reaction for 10-12 minutes, wherein the molar ratio of the formaldehyde to the melamine is (6.9-7.1): 1; 2, adjusting the pH value to 3-4, and carrying out a heat preservation reaction for 5-7 min, wherein the molar ratio of melamine to methanol is 1: (15-17), and carrying out negative pressure distillation at 65-70 DEG C; and 3, adjusting the pH value to 3-4, and carrying out a heat preservation reaction for 4-6 min, wherein the molar ratio of melamine to methanol is 1: (5-7), and then carrying out negative pressure distillation to 115-120 DEG C, and filtering to obtain the methylated melamine-formaldehyde resin. The method disclosed by the invention has the positive effects of avoiding the problem of quality difference of products among batches, and being easy to operate, good in product stability and high in yield.

Description

technical field [0001] The invention relates to the technical field of fine chemicals, in particular to a preparation method of methyl etherified melamine formaldehyde resin. Background technique [0002] Rubber adhesives are a very important class of methanol etherified melamine formaldehyde resins in amino resins. At present, apart from butanol-etherified melamine-formaldehyde resins for coatings, butanol-etherified melamine-formaldehyde resins have already matured, but methanol-etherified melamine-formaldehyde resins with a high degree of etherification (referred to as HMMM) are still in the development stage. The invention patent with application number 2020110369056 discloses a preparation method of methylated melamine formaldehyde resin, which adopts the reaction kettle-type batch reaction preparation method. This batch preparation method has product quality differences between batches The problem is that the process is cumbersome and inconvenient to operate. Conten...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G12/42C08G12/32
CPCC08G12/427C08G12/32
Inventor 马德龙石建明王庆振徐思明董玉灿马振宇温以亮王克军董瑞国王洪奎
Owner SHANDONG YANGGU HUATAI CHEM
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