Method for synthesizing highly-methylated amino resin through trimethylol melamine

A technology of trimethylol melamine and amino resin, which is applied in the field of environmental protection synthesis, can solve the problems of unfavorable environmental protection discharge, troublesome water treatment, increased treatment process and cost, etc., and achieves the advantages of reducing subsequent filtration requirements and costs, and reducing waste water treatment volume. Effect

Active Publication Date: 2017-11-17
CHONGQING JIANFENG HAOKANG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, because the above-mentioned synthetic method needs to use a large amount of lye, it causes a lot of trouble to the subsequent water treatment, increases the treatment process and cost, and is not conducive to environmental protection discharge.
In addition, the metal ions contained in the lye are also unfavorable for subsequent filtration

Method used

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  • Method for synthesizing highly-methylated amino resin through trimethylol melamine
  • Method for synthesizing highly-methylated amino resin through trimethylol melamine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Using trimethylol melamine as raw material to synthesize highly methylated amino resin:

[0030] (1) According to trimethylol melamine: the molar ratio of methyl alcohol is 1: 20 in above-mentioned reactor, drop into the methanol of above-mentioned metering, adjust reactor stirring frequency converter to 20Hz, add hydrochloric acid and adjust pH value to 3.5, add above-mentioned metering Trimethylol melamine, heating and regulating temperature is 55 ℃ and stirs to make it dissolve;

[0031] (2) after the completion of the reaction after the complete dissolution of trimethylol melamine, keep warm for 2 hours;

[0032] (3) feed ammonia into the reaction kettle through the above-mentioned ammonia gas feeding device, detect the pH value and adjust the pH to be 9;

[0033] (4) Start the vacuum pump, control the vacuum degree to 0.08MPa, the temperature is 60°C, and dealcoholize and dehydrate for 3h;

[0034] (5) Stop vacuuming, add butanol with a mass ratio of 20%, and sti...

Embodiment 2

[0037] Step is with embodiment 1, difference is as follows:

[0038] In step (1), the molar ratio of trimethylolmelamine:methanol is 1:10, the reactor is adjusted to stir the frequency converter to 30Hz, the pH value is adjusted to 5.0 by adding sulfuric acid, and the temperature is raised to 45°C for stirring and dissolving;

[0039] In step (2), keep warm for 1h;

[0040] In step (3), adjust the pH value to 8.0;

[0041] In step (4), the vacuum degree is controlled to 0.09MPa, the temperature is 80°C, and the time is 2h;

[0042] In step (5), 30% butanol was added and stirred for 40 min.

Embodiment 3

[0044] Step is with embodiment 1, difference is as follows:

[0045] In step (1), the molar ratio of trimethylolmelamine:methanol is 1:8, adjust the stirring frequency converter of the reactor to 10Hz, add hydrochloric acid to adjust the pH value to 6.0, and heat up and adjust the temperature to 35°C for stirring and dissolving;

[0046] In step (2), keep warm for 0.5h;

[0047] In step (3), the pH value is adjusted to 8.5;

[0048] In step (4), the vacuum degree is controlled to 0.1MPa, the temperature is 100°C, and the time is 0.5h;

[0049] In step (5), 40% butanol was added and stirred for 20 min.

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PUM

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Abstract

A method for synthesizing highly-methylated amino resin through trimethylol melamine includes the steps of putting methyl alcohol and trimethylol melamine in a reaction still in proportion, adding acid to adjust the pH value of a solution in the still, conducting heating and stirring till trimethylol melamine is completely dissolved, introducing ammonia gas into the reaction still to adjust and raise pH after keeping the temperature for a period of time, conducting dealcoholization and dehydration treatment to obtain a primary resin product, adding a butanol stabilizer to the primary resin product and stirring, and conducting filtering to obtain colorless viscous liquid, namely highly-methylated amino resin. Highly-methylated amino resin excellent in performance is obtained, the wastewater treatment amount is remarkably reduced, and production cost is reduced.

Description

technical field [0001] The invention relates to the environment-friendly synthesis of high methyl etherification amino resin. Background technique [0002] For the synthesis of etherified amino resins using melamine such as hexamethylolmelamine or tetramethylolmelamine, refer to the applicant’s previous patents or patent applications CN 103739563B, CN 103739803B, CN103709111B, CN105968283A, CN105968281A, CN105968282A and CN106008870A. In addition, CN106243300A and CN106349267A also disclose the synthesis method of etherified resin introduced by hybridization with flame retardant components. However, because the above synthetic method needs to use a large amount of lye, it causes a lot of trouble to the subsequent water treatment, increases the treatment process and cost, and is not conducive to environmental protection discharge. In addition, the metal ions contained in the lye are also unfavorable for subsequent filtration. Contents of the invention [0003] The object ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G12/42
CPCC08G12/425
Inventor 王文武胡劲松周建平张志轩
Owner CHONGQING JIANFENG HAOKANG CHEM
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