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Preparation method of high-imido and high-methoxylation melamine resin capable of being cured at low temperature

A high-etherified melamine and melamine technology, which is applied in the field of melamine resin preparation, can solve the problems of reduced imino content, increased temperature, and high product viscosity, and achieves increased hydroxyl value, low baking temperature, and simple process. Effect

Active Publication Date: 2017-02-22
重庆建峰新材料有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the higher the hydroxymethyl content, the lower the imino content, which increases the temperature required for the coating to be baked, and the product has a higher viscosity

Method used

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  • Preparation method of high-imido and high-methoxylation melamine resin capable of being cured at low temperature
  • Preparation method of high-imido and high-methoxylation melamine resin capable of being cured at low temperature
  • Preparation method of high-imido and high-methoxylation melamine resin capable of being cured at low temperature

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] (1) Put 90g of melamine and 30% formaldehyde solution into a four-necked flask according to the molar ratio of melamine: formaldehyde of 1:4.5, stir and adjust pH=9 with 10% NaOH and heat up to 50°C, after the melamine is completely dissolved keep warm for 2 hours;

[0026] (2) Then the system is cooled to below 35°C, methanol is added, and methanol is added according to the ratio of melamine: the molar ratio of methanol is 1:20, and the mixed solution with 37% hydrochloric acid: 88% formic acid volume ratio is 2: 1 to adjust the pH = 5. Keep warm for 2 hours after being transparent;

[0027] (3) After the etherification is finished, use 30% NaOH to adjust pH=9, carry out vacuum distillation at 80°C, finish distillation when the pressure is less than or equal to 1.0KPa after about 2 hours, add isobutanol to adjust product viscosity, and then Add 4% diatomaceous earth, stir evenly, and then suction filter until transparent.

Embodiment 2

[0029] (1) Put 90g of melamine and 30% formaldehyde solution into a four-neck flask according to the molar ratio of melamine:formaldehyde of 1:4.5, stir and adjust the pH to 9 with 10% NaOH; heat up to 55°C until the melamine is completely dissolved Keep warm for 90 minutes;

[0030] (2) Then cool down to below 35°C, add methanol, add methanol according to the ratio of melamine:methanol molar ratio of 1:20, adjust pH=4 with 37% hydrochloric acid: 88% formic acid mixed solution with a volume ratio of 3:1 , keep warm for 90 minutes after being transparent;

[0031] (3) After the etherification is finished, use 30% NaOH to adjust pH=9, carry out vacuum distillation at 80°C, finish distillation when the pressure is less than or equal to 1.0KPa after about 2 hours, add isobutanol to adjust product viscosity, and then Add 4% diatomaceous earth, stir evenly, and then suction filter until transparent.

Embodiment 3

[0033] (1) Put 90g of melamine and 30% formaldehyde solution into a four-necked flask according to the molar ratio of melamine: formaldehyde of 1:4.5, stir and adjust the pH to 9 with 10% NaOH; heat up to 45°C until the melamine is completely dissolved Keep warm for 3 hours;

[0034] (2) Then add methanol at 30°C, methanol is added according to the ratio of melamine:methanol molar ratio of 1:20, and the mixed solution with 37% hydrochloric acid:88% formic acid volume ratio of 1:3 is used to adjust pH=3 , keep warm for 45 minutes after being transparent;

[0035] (3) After the etherification is finished, use 30% NaOH to adjust pH=9, carry out vacuum distillation at 80°C, finish distillation when the pressure is less than or equal to 1.0KPa after about 2 hours, add isobutanol to adjust product viscosity, and then Add 4% diatomaceous earth, stir evenly, and then suction filter until transparent.

[0036] 2. Experimental results

[0037] 2.1 Determination results of formaldehyd...

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Abstract

The invention discloses a preparation method of a high-imido and high-methoxylation melamine resin capable of being cured at low temperature. According to the method, the high-imido and high-methoxylation melamine resin capable of being cured at low temperature is obtained by reacting melamine, a formaldehyde solution and methanol, paraformaldehyde is not required to be added, the step of synthesis of hydroxymethylation melamine as an intermediate product is omitted, preparation costs are reduced, links of crystallization, drying and the like of the intermediate product are omitted, energy consumption is low, a technological process is simple, the methanol only needs to be added at one step in reaction, and the preparation method is easy to control. In addition, a mixture of hydrochloric acid and formic acid is used as an etherification catalyst, and the effect of the obtained product is better than that of a single acid catalyst.

Description

technical field [0001] The invention relates to the technical field of preparation methods of melamine resins, in particular to a preparation method of low-temperature-curable high-imino and high-etherified melamine resins. Background technique [0002] High imino methyl etherified melamine resin can be widely used in various applications such as coil coatings, high-temperature coatings and water-based coatings. It is a good curing agent and cross-linking agent with good water solubility. Industrial quick bake varnish. Since the 1980s, my country began to develop methyl etherified melamine formaldehyde resins, focusing on monomeric melamine formaldehyde resins. At present, this type of resin is mainly based on hexahydroxy etherified resins, high imino high methyl ether resins with better performance Melamine formaldehyde resin is still dependent on imports. [0003] At present, the domestic preparation of high-imino high-etherified melamine-formaldehyde resin mainly contain...

Claims

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Application Information

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IPC IPC(8): C08G12/32
CPCC08G12/32
Inventor 郝小兰宫晓川池华春杨兴兵钟力杨振国刘婉贞高瑞
Owner 重庆建峰新材料有限责任公司
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