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Preparation method of melamino-formaldehyde resin with ultra-low formaldehyde content

A formaldehyde content, melamine technology, applied in the field of preparation of melamine formaldehyde resin, can solve the problem of reducing to 0.3% to 0.5%, achieve the effect of less acid consumption, short time and low reaction temperature

Active Publication Date: 2019-01-04
CHONGQING JIANFENG INDAL GROUP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Shi Yunming et al. (Modern Chemicals, 2006, 26 (S2): 247-248) have reported a method for removing free aldehydes in urea-formaldehyde resins, proposing to use inorganic ammonium salts, inorganic sodium salts, inorganic calcium salts and chlorinated sodium salts with Free formaldehyde reaction, but a large number of experiments show that this method can only reduce the free formaldehyde content in the resin to 0.3% ~ 0.5%

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] Add 2176g of methanol to a 5L flask, start a water bath to raise the temperature, and when it reaches (40-50)°C, add 1300g of hexamethylolmelamine to the flask, then add 30ml of concentrated hydrochloric acid, the hexahydroxymelamine gradually dissolves, and when the system Start timing after it is completely transparent, maintain the temperature, add 45ml of sodium hydroxide after 3.0 hours, and the pH value of the system is between 8.0 and 9.0. Then add 24ml of hydrogen peroxide, and add 36ml of sodium hydroxide. After the pH value of the system is stable, start to heat up and dealcoholize and dehydrate under reduced pressure. After the material temperature reaches 90°C, keep it warm for 1 hour, and then filter through diatomaceous earth to obtain the product.

[0050]The free aldehyde content of the product in Example 1 is 0.01%, the viscosity is 4500mpa.s, the appearance is a colorless transparent liquid, and the non-volatile matter content is 98.8%.

Embodiment 2

[0052] Add 1230g of methanol to a 3L flask, start a water bath to raise the temperature, and when it reaches (40-50)°C, add 735g of hexamethylolmelamine to the flask, then add 10ml of concentrated hydrochloric acid, and the hexahydroxymelamine gradually dissolves. After it is completely transparent, start timing, maintain the temperature, add 16ml of sodium hydroxide after 3.0 hours, and the pH value of the system is between 8.0 and 9.0. Then add 16ml of hydrogen peroxide, and add 25ml of sodium hydroxide. After the pH value of the system is stable, start to heat up and dealcoholize and dehydrate under reduced pressure. After the material temperature reaches 90°C, keep it warm for 1 hour, and then filter through diatomaceous earth to obtain the product.

[0053] The free aldehyde content of the product in Example 2 is 0.01%, the viscosity is 4600mpa.s, the appearance is a colorless transparent liquid, and the non-volatile matter content is 99.1%.

Embodiment 3

[0055] Add 1470g of methanol to a 3L flask, start a water bath to raise the temperature, and when it reaches (40-50)°C, add 735g of hexamethylolmelamine to the flask, then add 18ml of concentrated hydrochloric acid, and the hexahydroxymelamine gradually dissolves. After it is completely transparent, start timing and maintain the temperature. After 3.0 hours, add 30ml of sodium hydroxide. At this time, the pH value of the system is between 9.0 and 10.0. Then add 14ml of hydrogen peroxide, and add 24ml of sodium hydroxide. After the pH value of the system is stable, start to heat up and dealcoholize and dehydrate under reduced pressure. After the material temperature reaches 90°C, keep it warm for 1 hour, and then filter through diatomaceous earth to obtain the product.

[0056] The free aldehyde content of the product in Example 3 is 0.04%, the viscosity is 3900mpa.s, the appearance is a colorless transparent liquid, and the non-volatile matter content is 98.7%.

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Abstract

The invention discloses a preparation method of melamino-formaldehyde resin with the ultra-low formaldehyde content. The ultra-low formaldehyde content is 0.05 wt% lower than the free formaldehyde content in resin, and preferentially 0.01wt%. The method comprises the following steps of putting poly-hydroxymethyl melamine and methyl alcohol are put into a reactor, inorganic acid is added for a catalysis etherification reaction, and an inorganic base is adopted for terminating the etherification reaction; after the etherification reaction is terminated, an oxidizing agent is added, and alkali liquor is added in time so that the pH value is maintained between 8.0 and 10.0. According to the method, the free aldehyde content of amino resin is lowered to 0.05 wt% or less and even lowered to 0.01wt%, and other mass indexes meet requirements.

Description

technical field [0001] The invention belongs to the field of amino resins, and relates to a preparation method of melamine-formaldehyde resin with ultra-low formaldehyde content. Background technique [0002] The synthesis method of melamine formaldehyde resin is roughly divided into two types, one is one-step method, that is, the raw materials are put into the reaction kettle at one time, and the product is obtained by adjusting the process; the other is two-step method, that is, melamine and formaldehyde are mixed in alkaline Polymethylol melamine is produced under the conditions, and after drying, it undergoes etherification reaction with monohydric alcohol under acidic conditions to obtain the final product. [0003] When using the one-step method, a large amount of formaldehyde solution or solid formaldehyde will be used, so the formaldehyde content in the product is relatively high. In the later stage of the reaction, whether it is the formaldehyde solution method or ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G12/42C08G12/40
CPCC08G12/40C08G12/42
Inventor 杨振国钟力池华春
Owner CHONGQING JIANFENG INDAL GROUP
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