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Synthetic method of etherified amino resin

A technology of amino resin and synthesis method, which is applied in the chemical industry, organic chemistry, sustainable manufacturing/processing, etc., to achieve the effect of short process flow and less waste water

Active Publication Date: 2016-03-30
CHONGQING JIANFENG HAOKANG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The purpose of the present invention is to provide a method for synthesizing etherified amino resins with hexamethylol melamine and ethanol as raw materials for the deficiencies in the existing synthesis methods of etherified amino resins

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] A kind of method taking hexamethylol melamine as raw material synthetic mixed type highly etherified amino resin, concrete steps are as follows:

[0020] (1) According to the molar ratio of hexamethylolmelamine:ethanol as 1:6, put the ethanol measured above into the reaction kettle, adjust the speed of the agitator in the reaction kettle to 30 rpm, add 36% hydrochloric acid aqueous solution to adjust the pH value to 3.0 , adding the hexamethylolmelamine measured above, heating and adjusting the temperature to 30°C and stirring to dissolve it;

[0021] (2) After the hexamethylolmelamine is completely dissolved, the temperature rises to 40°C, and the reaction is kept for 30 minutes;

[0022] (3) Add 30% sodium hydroxide aqueous solution to neutralize the acidity in the system, adjust the pH to 8.0, and gradually raise the temperature to 90°C for dehydration under normal pressure;

[0023] (4) Start the vacuum pump, control the vacuum degree to 0.09MPa, and dehydrate at 7...

Embodiment 2

[0027] A kind of method taking hexamethylol melamine as raw material synthetic mixed type highly etherified amino resin, its specific steps are the same as embodiment 1, wherein:

[0028] In step (1), according to hexamethylolmelamine: ethanol molar ratio is 1: 8, add metered ethanol in the reaction kettle, adjust the stirring speed of the reaction kettle to be 50 rpm, add 36% hydrochloric acid aqueous solution to adjust the pH value 3.5, add the hexamethylolmelamine measured above, use 36% hydrochloric acid aqueous solution to keep the pH value at 3.5, and heat up to 35°C to dissolve it;

[0029] In step (2), heat up to 45°C for 45 minutes;

[0030] In step (3), adjust the pH value to 9.0;

[0031] In step (4), control the vacuum degree to 0.07MPa, and dehydrate at 80°C for 2 hours;

[0032] In step (5), add 3% diatomaceous earth and stir for 40 minutes;

[0033] In step (6), filter to obtain a colorless viscous liquid with a conversion rate of 78% (calculated as hexamethy...

Embodiment 3

[0035] A kind of method taking hexamethylol melamine as raw material synthetic mixed type highly etherified amino resin, its specific steps are the same as embodiment 1, wherein:

[0036] In step (1), according to hexamethylolmelamine: ethanol molar ratio is 1: 10, add the measured ethanol in the reaction kettle, adjust the stirring speed of the reaction kettle to be 70 rpm, add 36% hydrochloric acid aqueous solution to adjust the pH value 4.0, add the hexamethylolmelamine measured above, use 36% hydrochloric acid aqueous solution to keep the pH value at 4.0, and heat up to 40°C to dissolve it;

[0037] In step (2), heat up to 50°C for 60 minutes;

[0038] In step (3), adjust the pH to 10.0;

[0039] In step (4), control the vacuum degree to 0.06MPa, and dehydrate at a temperature of 100°C for 3 hours;

[0040] In step (5), add 5% diatomaceous earth and stir for 60 minutes;

[0041] In step (6), filter to obtain a colorless viscous liquid with a conversion rate of 80% (calc...

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Abstract

The invention relates to a synthetic method of etherified amino resin. The synthetic method comprises the following steps: putting hexamethylol melamine and ethyl alcohol in a reaction kettle in a certain proportion, adding acid so as to adjust the pH value to 3.0-4.0, heating to 40-55 DEG C, and performing heat-preservation reaction for 30-60 minutes; adding alkali to neutralize the acidity in the system so as to adjust the pH value to 8.0-10.0; starting a vacuum pump and performing dealcoholization and dehydration under a vacuum condition for 1-3 hours; stopping vacuum pumping, adding 2%-5% of diatomaceous earth, and stirring for 20-60 minutes; filtering to obtain a colorless viscous liquid, and packaging. According to the synthetic method of ether amino resin disclosed by the invention, the etherification degree of the obtained product is 10%-20% higher than that in a traditional synthetic method; the obtained etherified amino resin is stable in product performance and long in storage time; moreover, the synthetic method disclosed by the invention is short in technological process, few in produced waste water, energy-saving and environment-friendly.

Description

technical field [0001] The present invention generally relates to the field of chemical synthesis, in particular to a synthesis method of etherified amino resin. Background technique [0002] Etherified amino resins can be widely used in solvent-based decorative coatings, coil coatings, powder coatings, can coatings, high-solid coatings, water-based coatings, ink industry, paper industry, etc. The synthesis routes of traditional industrial etherified amino resins mainly include one-step one-bath method and one-step two-bath method. The former is first made into a melamine-formaldehyde initial condensation solution, and then etherified with alcohol. The latter is first made into a melamine initial contraction body, then concentrated and spray-dried at low temperature into a solid powder, and then etherified with alcohol. The latter is better in quality, but the process route is complicated and the investment is relatively large. The Chinese invention patent with the patent...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D251/70
CPCC07D251/70Y02P20/10
Inventor 胡劲松周建平肖波
Owner CHONGQING JIANFENG HAOKANG CHEM
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