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Phenyl phosphine diamide derivative as well as synthesis method and application thereof

A technology of phenylphosphine diamide and synthesis method, which is applied in the fields of nitrogen flame retardant materials and epoxy resins containing phosphorus, can solve problems such as application restrictions, and achieve the goal of avoiding phase separation, uniform and stable flame retardant effect, and ensuring uniform mixing Effect

Inactive Publication Date: 2018-10-16
FUJIAN CONSTR ENG GRP BUILDING MATERIAL SCI & TECH DEV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the use of phosphaphenanthrene-type flame retardants is limited due to its relatively expensive synthetic raw materials and preparation methods (requiring high-temperature reaction and solvent removal), so it is necessary to develop a kind of raw material that is relatively cheap and can recycle and reuse solvents. New Phosphorus and Nitrogen Flame Retardant Materials

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  • Phenyl phosphine diamide derivative as well as synthesis method and application thereof
  • Phenyl phosphine diamide derivative as well as synthesis method and application thereof
  • Phenyl phosphine diamide derivative as well as synthesis method and application thereof

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preparation example Construction

[0033] The present invention also relates to a method for synthesizing the above-mentioned phenylphosphine diamide derivatives, comprising the following steps:

[0034] (1) use phenylphosphine diacid chloride and primary amine as reaction raw materials, use tetrahydrofuran or diethyl ether as reaction solvent, and use triethylamine as reaction catalyst;

[0035] (2) the implementation of acylation reaction, primary amine is dissolved in ether or tetrahydrofuran, with triethylamine of equivalent amount as bottom material, slowly drip the ether or the tetrahydrofuran solution containing phenylphosphine dichloride under uniform stirring, The dripping time shall not be less than 2 hours;

[0036] (3) temperature of reaction is controlled below 5 ℃, after dripping finishes, continue stirring at room temperature for more than 5 hours to ensure that the reaction is complete;

[0037] (4) The product is filtered to remove triethylamine hydrochloride, and the solvent is recovered and ...

Embodiment 1

[0046] Synthesis of N,N'-diallyl-P-phenylphosphine diamide:

[0047] 0.1 mol of allylamine and 0.105 mol of triethylamine were dissolved in 100 mL of ether, placed in a 250 mL three-necked flask and stirred evenly; the ether solution of phenylphosphine dichloride (0.05 mol of phenylphosphine dichloride) was added dropwise to the flask under an ice-water bath. The acid chloride was dissolved in 50 mL of ether), and the dropwise addition time was 2 hours. After the dropwise addition was completed, stirring was continued at room temperature for 5 hours to complete the reaction. After the reaction was completed, the triethanolamine hydrochloride in the suspension was filtered off by suction filtration, and the filtrate was rotary evaporated to remove diethyl ether to obtain a crude product with a product yield of 94%. The product was washed 3 times with deionized water and dried for later use.

[0048] The purified product was tested and analyzed by the infrared spectrum of the ...

Embodiment 2

[0053] Flame Retardant Modification of Epoxy Resin Curing System by Phenylphosphine Diamide Derivatives:

[0054] Stir 100g of epoxy prepolymer with epoxy equivalent of 0.54 and 1-5g of phenylphosphine diamide derivative at 100°C for 5 minutes to mix thoroughly; add 33g of diaminodiphenylsulfone, and heat up to 130 ℃ Continue stirring until diaminodiphenyl sulfone is completely dissolved; then add the mixture into a preheated PTFE mold and cure at 160 ℃ for 1 hour, 180 ℃ for 2 hours, and 200 ℃ for 2 hours ; And prepare epoxy curable resin without adding phenylphosphine diamide derivative as blank sample under the same conditions.

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Abstract

The invention provides a phenyl phosphine diamide derivative as well as a synthesis method and application thereof. The synthesis method comprises the following steps: by taking phenyl phosphine oxalyl chloride and primary amine as reaction raw materials, tetrahydrofuran or diethyl ether as reaction solvents, and triethylamine as a reaction catalyst, dissolving the primary amine into ethyl ether or tetrahydrofuran, and by taking triethylamine as an equal mass as a substrate, slowly dropping a phenyl phosphine oxalyl chloride containing ethyl ether or tetrahydrofuran solution while stirring ata uniform speed, wherein the dropping time is longer than 2 hours; controlling a reaction temperature to be below 5 DEG C, and continuously stirring for more than 5 hours at the room temperature afterdropping is completed; filtering a product to remove triethylamine hydrochloride, carrying out vacuum distillation, and washing an obtained product with deionized water, so as to obtain a crude product. The product can be applied to flame-retardant modification on an epoxy resin. The product provided by the invention can be used as a flame-retardant modifier, meanwhile is low in synthesis raw material price, simple and gentle in synthesis process and low in solvent melting point in a reaction process and can be recycled and repeatedly used, and energy consumption is correspondingly reduced.

Description

【Technical field】 [0001] The invention relates to the technical field of epoxy resin-based phosphorus- and nitrogen-containing flame-retardant materials, in particular to a phenylphosphine diamide derivative and a synthesis method and application thereof. 【Background technique】 [0002] As a widely used thermosetting material, epoxy resin is widely used in electronic appliances, engineering building materials, home furnishings and other fields due to its excellent electrical insulation properties, corrosion resistance and adhesive properties, but its flammability has always suffered Criticism: Once ignited, it is difficult to self-extinguish and accompanied by falling objects with flames, it may ignite the surrounding combustibles and cause the fire to spread, causing great losses to life, property and safety. Traditional halogen-based flame retardants have a significant flame retardant effect on epoxy resins, but they will release toxic gases such as hydrogen halide during ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/44C07F9/6521C08K5/5399C08L63/00
CPCC07F9/4419C07F9/4469C07F9/4476C08K5/5399C08L2201/02C08L63/00
Inventor 沈航黄春文林顺官郑敏升
Owner FUJIAN CONSTR ENG GRP BUILDING MATERIAL SCI & TECH DEV
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