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Synthetic method of nitrogen-containing flame-retardant phenolic resin

A technology of phenolic resin and synthesis method, which is applied in the field of preparation of modified phenolic resin, can solve problems such as increased process complexity, cumbersome process, and influence on product electrical properties, and achieves the effects of reasonable molecular weight distribution, simple operation, and convenient implementation

Inactive Publication Date: 2008-12-17
北京新福润达绝缘材料有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For the synthesis of nitrogen-containing and nitrogen-containing flame-retardant phenolic resins, a two-step method is usually used. The process is relatively cumbersome, and inorganic bases are used in the synthesis process, and extraction methods are required to separate and remove inorganic metal ions in the system. The subsequent reaction temperature needs to be Reaching 170°C further increases the complexity of the process and affects the electrical properties of the product

Method used

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  • Synthetic method of nitrogen-containing flame-retardant phenolic resin
  • Synthetic method of nitrogen-containing flame-retardant phenolic resin
  • Synthetic method of nitrogen-containing flame-retardant phenolic resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Embodiment 1: Methylmelamine / formaldehyde / guanidine carbonate / p-phenylphenol prepares nitrogen-containing flame-retardant phenolic resin

[0035] In a 1000ml three-necked flask equipped with stirring, take by weighing 140 grams of methyl melamine by weight, 100 grams by weight of 100 wt% acetaldehyde solution, add 250 g of water and stir evenly, then adjust the pH of the solution with 15 wt % guanidine carbonate aqueous solution The value is 8.5, the temperature is raised to 70°C, and the temperature is maintained at 70-75°C for 40 minutes. Subsequently, add 108 gram parts by weight of p-cresol and 120 gram parts by weight of 100wt% acetaldehyde solution, adjust the pH value of the solution to 9.0 with 15wt% guanidine carbonate aqueous solution, heat up to 70°C, keep the temperature at 70~75°C React for 40 minutes. Continue to use 15wt% guanidine carbonate aqueous solution to adjust the pH of the solution to 9.5, raise the temperature to 80° C., and keep the temperatur...

Embodiment 2

[0037] Embodiment 2: Methylmelamine / formaldehyde / guanidine carbonate / p-phenylphenol prepares nitrogen-containing flame-retardant phenolic resin

[0038] In the 1000ml there-necked flask with stirring, take by weighing the methyl melamine of 140 gram parts by weight, the 37wt% formaldehyde solution of 240 gram parts by weight, after stirring evenly, adjust the pH value of solution with 10wt% guanidine carbonate aqueous solution to be 10.0, Raise the temperature to 65°C and keep the temperature between 65°C and 70°C for 60 minutes. Add the phenylphenol of 170 grams by weight and the 37wt% formaldehyde of 260 grams by weight, adjust the pH value of the solution with 20wt% guanidine carbonate aqueous solution to be 9.5, heat up to 75°C, keep the temperature between 75~80°C for reaction 80 minutes. The pH value of the solution was adjusted to 9.5 with 15 wt % guanidine carbonate aqueous solution, the temperature was raised to 85° C., and the temperature was kept between 85° C. and 9...

Embodiment 3

[0040] Embodiment 3: Preparation of nitrogen-containing flame-retardant phenolic resin by benzomelamine / formaldehyde / aminoguanidine / p-phenylphenol

[0041] In the 1000ml there-necked flask that is equipped with stirring, take by weighing the benzomelamine of 187 gram parts by weight, the 37wt% formaldehyde aqueous solution of 200 gram parts by weight, after stirring evenly, adjust the pH value of solution with 10wt% aminoguanidine aqueous solution to be 10.0, Raise the temperature to 80°C and keep the temperature between 80-85°C for 30 minutes. Add 170 gram parts by weight of p-phenylphenol and 220 gram parts by weight of 37wt% formaldehyde, adjust the pH value of the solution to 10.0 with 10wt% aminoguanidine aqueous solution, heat up to 85°C, and keep the temperature between 85~90°C React for 60 minutes. The pH value of the solution was adjusted to 10.0 with 10 wt % guanidine carbonate aqueous solution, the temperature was raised to 90° C., and the temperature was maintaine...

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Abstract

The invention pertains to the technical field of preparing a modified phenolic resin and particularly relates to a synthetic method of a nitrogen-containing and flame-retarding phenolic resin; the synthetic method of the invention comprises the following steps: the monosubstituted melamine monomer and the aldehyde monomer with a mole ratio of 1:2 to 5 are blended and put in to an organic base adjusting solution system with the pH value of 8 to 11 to carry out a hydroxymethylation at a temperature of 65 DEG C to 90 DEG C; the para-orienting organic phenol monomer and the aldehyde monomer with mole ratio of 1:2 to 5 are added into the reaction system; the hydroxymethylation lasts for 0.5 hours to 2 hours at a temperature of 65 DEG C to 90 DEG C; then a condensation polymerization is carried out at the temperature of 75 DEG C to 100 DEG C; an organic solvent is added for the purpose of pressure reduction and azeotropy; the reflow temperature is kept at 60 DEG C to 80 DEG C; after the moisture in the reaction system is removed, an organic solvent is added to dilute, prepare and obtain nitrogen-containing and flame-retarding phenolic resin with a thiotrzinone structure unit, which can be used for producing non-halogen and flame-retarding phenolic resin laminates of grade FV0 and applied as epoxy resin hardeners.

Description

technical field [0001] The invention belongs to the technical field of preparation of modified phenolic resins, in particular to a synthesis method of nitrogen-containing flame-retardant phenolic resins. Background technique [0002] With the increasingly stringent fire safety standards at home and abroad and the rapid growth of the amount of polymer materials, while improving the flame retardant performance of organic polymer materials, paying more attention to environmental protection and ecological safety has become an important trend of flame retardant technology and its development. Combustion agent has become one of the important additives of polymer materials and composite materials. It is estimated that the total consumption of flame retardants in the world in 2003 has reached more than 1.2 million tons per year, of which 85% are additive flame retardants and 15% are reactive flame retardants. It is estimated that the total consumption of flame retardants in the wor...

Claims

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Application Information

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IPC IPC(8): C08G8/28C08G12/38
Inventor 王楠于存海王德生周长琰
Owner 北京新福润达绝缘材料有限责任公司
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