Flame-retardant compound, preparation method and application thereof

A technology of compounds and flame retardants, applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, organic chemistry, etc. cracks and other problems, to achieve the effect of low dielectric loss, excellent dielectric constant, and reduce electron migration

Active Publication Date: 2019-03-26
ELITE ELECTRONICS MATERIAL ZHONGSHAN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, the use of halogen flame retardants is restricted due to environmental pressure
In addition, commonly used phosphazene compounds (such as SPB-100 produced by Otsuka Chemical) or condensed phosphoric acid esters (such as PX-200 produced by Daihachi Chemical) have problems such as low melting point, low thermal decomposition temperature, and high-temperature freeness. The thermal expansion coefficient of the substrate produced by it is relatively large, which may easily cause inner layer cracks during the circuit board manufacturing process, thereby reducing the process qualification rate

Method used

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  • Flame-retardant compound, preparation method and application thereof
  • Flame-retardant compound, preparation method and application thereof
  • Flame-retardant compound, preparation method and application thereof

Examples

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preparation example Construction

[0075] The present invention further provides a preparation method of the compound, comprising reacting the phosphorus-containing compound with solid phosgene or phosgene.

[0076] Specifically, the aforementioned manufacturing method is to react the phosphorus-containing compound with solid phosgene or phosgene in a solvent under reflux; the reflux time can be between 1 hour and 10 hours, preferably between 2 hours and 10 hours, For example, between 4 hours and 8 hours; the reaction temperature of heating to reflux is between 50°C and 200°C, preferably between 50°C and 120°C, such as between 70°C and 120°C.

[0077]In a preferred embodiment, the molar ratio of phosphorus-containing compound to solid phosgene or phosgene is between 12:1 and 1:1, preferably between 10:1 and 3:1, for example 10:1 and Between 4:1, 10:1 and 5:1.

[0078] In a preferred embodiment, the solvent is toluene (TL), dimethylacetamide (DMAC), dimethylformamide (DMF), 2-propanol methyl ether (PM), propyle...

preparation example 1

[0153] Preparation Example 1: Preparation of Formula (IV) Compound

[0154] Insert a thermometer and a condenser into a 2000 ml three-necked flask, then add 1000 ml of toluene and 0.9 moles (about 195 grams) of DOPO, heat (about 80°C) and stir to dissolve until clear and transparent. Then the solid phosgene (0.1 mol, 29.8 g) dissolved in toluene is transferred to the constant pressure funnel, slowly dripped into the flask under the protection of nitrogen, and heated to the boiling point of the solvent or to a temperature above the boiling point (for example, 120° C. ) for reflux reaction. After reacting for 6 hours, it was cooled to room temperature, filtered, and vacuum-dried to obtain a white powder with a yield of 92.5%.

[0155] With reflective Fourier transform infrared spectroscopy (Fourier transform infrared spectroscopy, FTIR) analysis of the resulting white powder, the analysis results are as follows Figure 1A and 1B shown. Among them, by Figure 1A It can be seen...

preparation example 2

[0156] Preparation example 2: preparation of formula (V) compound

[0157] In a 2000 ml three-necked bottle, insert a thermometer and a condenser tube, add 1000 ml of toluene and 1 mole (about 202 g) of DPPO, heat (about 80°C) and stir to dissolve until clear and transparent. Then the solid phosgene (0.1 mol, 29.8 g) dissolved in toluene was transferred to a constant pressure funnel, and slowly dropped into the flask under nitrogen protection for reflux reaction (solvent boiling point or temperature above boiling point, for example 120° C.). After reacting for 6 hours, it was cooled to room temperature, filtered, and vacuum-dried to obtain a white powder with a yield of 91.5%.

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Abstract

The invention discloses a phosphorus-containing compound. The phosphorus-containing compound can be used as a flame retardant, can be matched with other components to prepare a resin composition for manufacturing articles such as prepregs, resin films, resin films adhered by copper foils, laminated boards or printed circuit boards and the like, so that improvement is made in the aspects of glass transition temperature, thermal expansion coefficient, heat resistance, flame retardance, dielectric constant and dielectric loss and the like. In addition, the invention also discloses a preparation method of the phosphorus-containing compound and the resin composition containing the compound.

Description

technical field [0001] The present invention relates to a compound, its preparation method, resin composition and articles made thereof, especially to a kind of prepreg, resin film, resin film with copper foil, laminate (such as copper foil substrate) And compounds for printed circuit boards, their preparation methods and applications. Background technique [0002] Printed circuit boards are used in a wide range of applications, such as industrial large-scale computers, communication instruments, electrical measuring devices, defense and aviation products, and civilian electrical products, etc. Most of them require printed circuit boards as the basis for carrying various electronic components. With the advancement of science and technology, various electronic products are developing rapidly in terms of miniaturization, multi-function, high performance and high reliability. Therefore, printed circuit boards are also gradually developing towards high precision, high density, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/40C07F9/53C07F9/6574C08L71/12C08L79/04C08L79/08C08K5/5357C08K5/5397C08K5/5333
CPCC07F9/4084C07F9/5325C07F9/657181C08K5/5357C08L71/126C08L2201/02C08L2205/025C08L2205/035C08L79/04C08L79/08C08K5/5397C08K5/5333C07F9/5329C07F9/4025C08K5/0066C08K5/5313G01N2021/3595C07F9/304G01N25/4866G01R33/46C07F9/4034
Inventor 胡志龙林立成
Owner ELITE ELECTRONICS MATERIAL ZHONGSHAN
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