Low Dielectric Phosphorous Flame Retardant Hardener and Its Application

A low-dielectric, hardener technology, applied in coatings, fire-resistant coatings, epoxy resin coatings, etc., can solve the problems of low moisture absorption, reduce hardening bridging density, insufficient flame retardancy, etc., and achieve good flame retardancy , excellent flame retardancy and thermal stability

Active Publication Date: 2019-09-27
NANYA PLASTICS CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Phosphorus-containing epoxy resin is a reactive flame retardant, and the halogen-free copper-clad laminate made of it has good comprehensive performance. However, with environmental regulations such as ROHS and POHS, lead-containing environmentally hazardous substances are banned, making printed circuit boards Assembling needs to increase the soldering temperature. Therefore, there are increasing expectations for flame-retardant polymers with high heat resistance, thermal stability, low moisture absorption, and high adhesion to the upstream materials, and the formulation system with phenolic resin as the hardener has excellent performance. The heat resistance has been maturely used in the lead-free process of printed circuit boards, in which the phenolic resin hardener accounts for about 20-40% by weight of the formula, which results in insufficient phosphorus content and flame retardancy in the formula of phosphorus-containing epoxy resin. Insufficient problem, in order to solve the aforementioned problem, more phosphorus content is introduced into the synthesis reaction to ensure flame retardancy, which instead leads to an increase in molecular weight and a decrease in hardened bridging density, insufficient Tg of the hardened product, and degradation of thermal properties, which cannot meet the requirements of printed circuit boards. Require

Method used

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  • Low Dielectric Phosphorous Flame Retardant Hardener and Its Application
  • Low Dielectric Phosphorous Flame Retardant Hardener and Its Application
  • Low Dielectric Phosphorous Flame Retardant Hardener and Its Application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 0

[0034] Example 0 Synthesis of low dielectric phosphorous-containing hardener of the present invention:

[0035] (1) Synthesis of 2,6-dimethylphenol phenolic resin compound resol: 121.5g (1 mole) 2,6-dimethylphenol, 97.2g 92% paraformaldehyde (3 moles), 800g pure water, 5.7 g 49.5% aqueous sodium hydroxide solution was placed in a 1000ml reaction tank, and reacted at 45°C for 20 minutes under heating and stirring. Then add 30g of 10% sulfuric acid aqueous solution to neutralize, add 230g of MIBK solvent to dissolve, drain off the water layer after liquid separation, then use 200g of pure water to wash twice, take the MIBK layer to obtain 2,6-dimethylphenol novolac resin compound A total of 440 g of the MIBK solution, with a yield of 80% (analyzed by HPLC), yielded 0.75 moles of 2,6-dimethylphenol novolac resin compound resol.

[0036] (2) Synthesis of bisphenol A grafted with 1 mole of 2,6-dimethylphenol novolac resin (BDP for short): Dissolve 228g (1 mole) of bisphenol A in 2...

Embodiment 1-3

[0043]Use the low-dielectric phosphorus-containing flame-retardant hardener of the present invention to apply to glass fiber laminated boards, and have excellent flame retardancy, heat resistance and low dielectric constant resin varnish (Varnish) formulation composition, and its formulation composition is detailed in Table 1. , using a solvent such as propylene glycol monomethyl ether (PM) or methyl ethyl ketone or acetone to adjust the resin varnish (Varnish) formulation composition with a solid content of 65%, prepare a glass fiber laminate with a known method, impregnate 7628 glass fiber cloth with the above resin liquid, and then dry at 170°C (impregnation machine temperature) for a few minutes. By adjusting and controlling the drying time, the minimum melt viscosity of the dried prepreg can be adjusted to be between 4000-10000poise. Finally, 8 prepregs are stacked layer by layer. Between two 35μm thick copper foils, at 25kg / cm 2 Under pressure, control the heating progra...

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Abstract

The invention provides a phosphorus-containing flame-retardant hardener with excellent flame retardance and heat resistance and a low dielectric constant. The molecular structure of the phosphorus-containing flame-retardant hardener is shown in the formula 1 in the description, wherein n is a mean value ranging from 0 to 2, m is a mean value ranging from 0 to 1, y is a mean value ranging from 0 to 2, and x is a mean value ranging from 0 to 10. By adding the phosphorus-containing flame-retardant hardener into a glass fiber laminate formula, the UL-94V0 flame retardance requirement can be met, the dielectric constant reaches 4.0 (1 GHz), and a pressure cooking test (PCT) shows that through soldering tin dipping at 288 DEG C after 2 h of water absorption, the heat resistance lasts for 10 min or longer without laminate blasting. The prepared flame-retardant hardener can serve as a raw material for synthesizing epoxy resin and cyanate ester resin or serve as a hardener of epoxy resin, and can be applied to insulating materials or adhesives or coatings of copper-clad laminates or EMC packages or other electronic assemblies with a high reliability requirement.

Description

technical field [0001] The invention is a novel low-dielectric halogen-free phosphorus-containing phenolic resin compound. The phosphorus-containing phenolic resin compound is applied to glass fiber laminates, exhibits good flame retardancy, low dielectric and heat resistance, and is suitable for high-performance printed circuits board use. Background technique [0002] In the past, in the flame retardant technology of epoxy resin, when synthesizing epoxy resin or formulating epoxy resin composition formula to introduce or add halogen compounds (such as tetrabromobisphenol A) to impart flame retardant properties, brominated epoxy resin has excellent Flame retardant properties, so it is widely used in electronic materials that require flame retardant properties, but the use of halogen flame retardants will release hydrogen bromide, tetrabromobiphenyldioxin and tetrabromobibenzofuran during combustion, which are corrosive Phosphorus and toxic carcinogens have been gradually b...

Claims

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Application Information

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Patent Type & AuthorityPatents(China)
IPC IPC(8): C08G59/62C08G8/28C09D163/00C09D5/18
Inventor李政中吴振华
OwnerNANYA PLASTICS CORP