Hydroxymethylated melamino-formaldehyde resin, preparation method and application thereof

A technology of methylolated melamine and formaldehyde resin, which is applied in the field of preparation of methylolated melamine-formaldehyde resin powder, can solve the problem of reducing the methylol content of methylolamine resin, difficult to separate methylolamine resin, and high yield Only 30% of the problem, to achieve the effect of enhancing mechanical properties, easy to popularize, and suppress droplet

Inactive Publication Date: 2019-12-31
XIHUA UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the reported preparation method has the following disadvantages: (1) during the preparation process, due to the unavoidable increase in temperature and decrease in pH value, the methylolated melamine formaldehyde resin is easily cross-linked and cured, thereby reducing the amount of methylolamine Methylol Content in Resin
(2) Since the methylolamine resin solution contains a large amount of hydrogen bonds, it is difficult to separate all the methylolamine resins by the above method, so that the yield is lower
It is mentioned in Chinese patent "201010122554.0" that its yield is only 30%
However, there are no relevant reports on the direct use of methylolamine resin in the preparation of polymer composites to enhance the mechanical properties and carbon-forming properties of materials.

Method used

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  • Hydroxymethylated melamino-formaldehyde resin, preparation method and application thereof
  • Hydroxymethylated melamino-formaldehyde resin, preparation method and application thereof
  • Hydroxymethylated melamino-formaldehyde resin, preparation method and application thereof

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preparation example Construction

[0031] The first technical problem to be solved in the present invention is to provide a method for preparing methylolated melamine formaldehyde resin powder with high methylol content and high yield. The preparation process comprises the following steps:

[0032] (1) First add melamine and 37% formaldehyde solution into the reaction flask at a molar ratio of 1:2 to 1:7, then add distilled water to keep the theoretical solid content at 10 to 50%; then, control the reaction temperature to 40°C ~95°C, stir and react for 0.5~6h. The whole reaction process needs to use alkali solution to control the pH value of the system to be 8-11;

[0033] (2) After the reaction is over, put the reaction solution into a quick-freezing refrigerator or liquid nitrogen, and freeze it into solid ice cubes;

[0034] (3) Then, freeze-dry or supercritically dry the solid ice cubes; obtain methylolated melamine-formaldehyde resin powder with a yield as high as 95%.

Embodiment 1

[0037] Add 126g (1mol) of melamine and 243g (3mol) of 37% formaldehyde solution into the reaction flask, then add 864g of distilled water to make its theoretical solid content 20%; then, use 10% mass concentration of sodium hydroxide solution to adjust the pH value of the solution , keep the pH value of the whole reaction process at 9; stop the reaction after reacting at 85° C. for 1.5 h, quickly freeze the reaction solution into ice cubes, and freeze-dry to obtain methylolated melamine formaldehyde resin powder. The actual solid content of the obtained methylolated melamine formaldehyde resin (solid content=methylolated melamine resin powder / hydroxylated melamine resin solution) is 19.5%, the yield is 98%, the initial decomposition temperature is 148 ° C, and the storage stability after redissolving up to 60 days.

Embodiment 2

[0039] Add 63g (0.5mol) of melamine and 243g (3mol) of 37% formaldehyde solution into the reaction flask, then add 612g of distilled water to make its theoretical solid content 20%; then, use 10% mass concentration of sodium hydroxide solution to adjust the pH of the solution Value, keep the pH value of the whole reaction process at 9; stop the reaction after reacting at 85°C for 1.5h, freeze the reaction solution into ice cubes, and freeze-dry to obtain methylolated melamine formaldehyde resin powder. The actual solid content is 18.7%, the yield is 96%, the initial decomposition temperature is 98°C, and the storage stability after reconstitution reaches 10 days.

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Abstract

The invention relates to the technical field of fine chemicals and flame-retardant materials, in particular to a preparation method and application of hydroxymethylated melamino-formaldehyde resin powder. The preparation method of the hydroxymethylated melamino-formaldehyde resin includes the steps of: (1) firstly adding melamine and a formaldehyde solution into a reaction container, then adding distilled water to keep the solid content of the system at 10-50%, then controlling the reaction temperature at 40DEG C-95DEG C, and carrying out stirring reaction for 0.5-6h; (2) at the end of the reaction, freezing the reaction container containing the reaction solution to convert the reaction solution into a solid reactant; and (3) finally, drying the obtained solid reactant to obtain the hydroxymethylated melamino-formaldehyde resin powder. The hydroxymethylated melamino-formaldehyde resin prepared by the preparation method of the hydroxymethylated melamino-formaldehyde resin provided by the invention has the characteristics of high hydroxyl content and high yield.

Description

technical field [0001] The invention relates to the technical fields of fine chemicals and flame-retardant materials, in particular to a preparation method and application of methylolated melamine-formaldehyde resin powder. Background technique [0002] By controlling the reaction conditions of melamine and formaldehyde, methylolamine resin, methyl ether amine resin and methylene amine resin can be obtained respectively. Methylolamine resin has good water solubility and is easy to self-crosslink and solidify. It is often used as a finishing agent for fabrics and papers, endowing them with waterproof, shrink-proof and wrinkle-proof functions. At present, methods such as crystallization, centrifugation, and evaporative drying are commonly used in industry to remove the moisture in the solution of methylolated melamine formaldehyde resin (abbreviated as methylolamine resin) to obtain its powder, such as Chinese patent "201010561762.0", "201010122554.0 ", "2016104656216", "2018...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G12/32C08J5/18C08L61/28C08L75/08C08L63/00C08L23/12C08K3/32
CPCC08G12/32C08J5/18C08L63/00C08L23/12C08J2375/08C08J2461/28C08L2201/02C08K2003/323C08L61/28C08K3/32
Inventor 陈明军刘幸雅汪婷叶桃萍黄保桃肖瑶
Owner XIHUA UNIV
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