Phosphorus-containing flame retardant composition, and phosphorus-containing polyphenyl ether resin composition, prepreg and laminated board using the same

A flame retardant composition, polyphenylene ether resin technology, applied in the directions of synthetic resin layered products, layered products, metal layered products, etc., can solve the problems of high melting point, reduced heat resistance, and strong plasticity.

Active Publication Date: 2015-07-15
GUANGDONG SHENGYI SCI TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For a long time, those skilled in the art have studied thermosetting cyanate esters, bismaleimide resins, hydrocarbon resins, etc. with good dielectric properties; in addition, polyphenylene ether resins have good dielectric properties, Heat resistance has also been studied as a high-frequency and high-speed material by many technicians, but due to its high melting point and poor fluidity, it is subject to many restrictions in application, and the melt viscosity of prepregs is large, which cannot meet the requirements of multi-layer printing. Process requirements for circuit boards
By reducing the molecular weight of polyphenylene ether resin, it can effectively reduce its melting temperature and improve fluidity, but this also sacrifices the heat resistance of polyphenylene ether resin
[0004] CN1745142A uses a polyphenylene ether resin whose end group contains vinylphenyl and m-vinylphenyl as the main resin, uses trienyl isocyanurate as a crosslinking curing agent, and can also add inorganic fillers and flame retardants if necessary Obtain a polyphenylene ether resin composition, and then impregnate NE type glass fiber fabrics to obtain prepregs and laminates with excellent dielectric properties and higher glass transition temperatures, but due to the use of isocyanurate in the composition Acid trienyl ester is used as a cross-linking curing agent, its molecular weight is low, and it is very easy to volatilize during the prepreg production process, which is not conducive to the stable production of prepregs and laminates
[0006] WO2006/023371A1 provides a composition of a bifunctional polyphenylene ether resin and an unsaturated olefin monomer, which can improve the fluidity and cured properties of the polyphenylene ether resin, but does not point out that the bifunctional polyphenylene ether resin Performance advantages when used in the field of laminated boards, and the unsaturated olefin monomers used are low molecular weight compounds, which are easy to volatilize at high temperature

Method used

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  • Phosphorus-containing flame retardant composition, and phosphorus-containing polyphenyl ether resin composition, prepreg and laminated board using the same
  • Phosphorus-containing flame retardant composition, and phosphorus-containing polyphenyl ether resin composition, prepreg and laminated board using the same
  • Phosphorus-containing flame retardant composition, and phosphorus-containing polyphenyl ether resin composition, prepreg and laminated board using the same

Examples

Experimental program
Comparison scheme
Effect test

Synthetic example 1

[0096] Synthesis Example 1: Preparation of DOPO Derivatives

[0097] Add potassium tert-butoxide 230g in the four-neck reactor equipped with addition funnel, thermocouple, mechanical stirrer and nitrogen flow, solvent anhydrous DMSO1.5L. The mixture was stirred at room temperature until it became a homogeneous solution. The solution was cooled to 10°C, and DOPO 42.3g was added in 10 small portions to keep the reaction temperature below 30°C. Slowly add 92 g of dichloroethane in the addition funnel to the above solution within 1 hour. Heated to 50°C for 1 hour. Cool to 10°C to react and add 3 L of water. The slurry was filtered and the wet cake was washed with water, acetone ethyl acetate to give 532 g of crude wet material which was refluxed in MeCN / ethanol / water 5320 ml and cooled slowly to 5°C. Filter the white solid through a funnel, and dry it in a vacuum oven at 80°C for 8 to 10 hours to obtain 260 g of a dry white powder, which is DOPO derivative 1 of formula (1), wh...

Synthetic example 2

[0099] The synthetic method is with reference to Synthetic Example 1, and dichloromethane is replaced with dichloro-p-xylene, obtains the DOPO derivative 2 of formula (1), wherein R 1 For phenyl.

[0100] Mixing example 1: Preparation of phosphorus-containing flame retardant composition (P15.4%)

[0101] 35 parts by weight of the hypophosphite compound, 100 parts by weight of the DOPO derivative of Synthesis Example 1 and 18 parts by weight of the polyphosphazene compound were mixed to obtain a phosphorus-containing composition;

[0102] Described hypophosphite compound is:

[0103]

[0104] The polyphosphazene compound has the following structure:

[0105] Wherein R is a methyl group, and wherein n is an integer of 3-100.

[0106] Mixing example 2: Preparation of phosphorus-containing composition (P16%)

[0107] The hypophosphite compound of 50 parts by weight, the DOPO derivative of Synthetic Example 1 of 100 parts by weight and the polyphosphazene compound of 25 pa...

Embodiment 1

[0128] Mix 100g of methyl methacrylate-modified polyphenylene ether SA9000 with toluene as a solvent, dissolve completely to obtain an end-group functionalized polyphenylene ether resin solution, and then add 45g of styrene-butadiene copolymer R100 as a crosslinker agent, add 2g dicumyl peroxide as initiator, 45g mixing example 1 phosphorus composition as flame retardant, 0.8g epoxy silane coupling agent and 80g silicon dioxide (SC-2050SQ) as filler, The above mixture was mixed in toluene, stirred and dissolved to obtain a uniform resin composition, ie glue.

[0129] Impregnate the above-prepared glue into the E-glass fiber cloth, heat and dry at 155°C for 3-10 minutes, and completely evaporate the solvent to obtain a prepreg. Copper foils with a thickness of 35 μm were attached to both sides of the 8-ply prepreg prepared above, and hot-pressed at a temperature of 200 ° C and a pressure of 3.0 MPa for 90 minutes to obtain a double-sided copper-clad laminate.

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PUM

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Abstract

The invention provides a phosphorus-containing flame retardant composition, including: a hypophosphite compound, a DOPO derivative and a polyphosphazene compound. The composition as a flame retardant can play a synergistic effect of several phosphorus-containing compounds, realizes halogen-free flame retardance under small addition amount and reaches level V-0. The invention also provides a contains a polyphenyl ether resin composition containing the above phosphorus-containing flame retardant compositions and a prepreg and a copper clad laminated board prepared from the same. After curing, the polyphenyl ether resin composition achieves flame retardance of V-0 grade under the condition to which the halogen flame retardant does not apply and keeps good dielectric property and heat resistance of polyphenyl ether resin; the prepreg and copper clad laminated board made from the composition have good dielectric property and heat resistance, and realize halogen-free flame retardance to UL 94-V0 grade while ensuring excellent heat resistance and dielectric property; and the composition is applicable to the field of high speed and high frequency printed circuit board, and is in line with the future requirements of green and environmental protection.

Description

technical field [0001] The invention belongs to the technical field of copper-clad laminates, and relates to a phosphorus-containing composition, a phosphorus-containing polyphenylene ether resin composition, a prepreg and a laminate using the composition. Background technique [0002] In recent years, with the development of high-performance, high-functionality and networking of computers and information communication equipment, in order to transmit high-speed and process large-capacity information, the operating signal tends to be high-frequency, so the material of the circuit board is required. In particular, there is a rapid development in those electronic devices using broadband such as mobile communication devices. [0003] Among conventional printed circuit board materials, epoxy resins excellent in adhesive properties are widely used. However, epoxy resin circuit substrates generally have high dielectric constant and dielectric loss tangent (dielectric constant is g...

Claims

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Application Information

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IPC IPC(8): C08L85/02C08L71/12C08K5/5313C08K3/36B32B27/04B32B27/18B32B27/28B32B15/08B32B15/20H05K1/03
CPCB32B15/08B32B15/20B32B27/04B32B27/18B32B27/28C08K3/36C08K5/5313C08L71/12C08L85/02H05K1/03
Inventor 曾宪平陈广兵关迟记杨文华何烈相
Owner GUANGDONG SHENGYI SCI TECH
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