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Environment-friendly preparation method of phosphorus flame retardant, namely 2-(diphenylphosphinoyl)-1, 4-benzenediol

A technology of diphenylphosphono and phosphorus-based flame retardants, applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, organic chemistry, etc., can solve the problem of low product yield and complicated purification process , high toxicity and other problems, to achieve the effect of high yield, simple purification and less by-products

Inactive Publication Date: 2013-09-25
QINGDAO FUSILIN CHEM SCI & TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In order to overcome the defects of high toxicity, complex purification process and low product yield in the synthesis process of flame retardant 2-(diphenylphosphono)-1,4-benzenediol, the present invention provides a new environmentally friendly Preparation

Method used

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  • Environment-friendly preparation method of phosphorus flame retardant, namely 2-(diphenylphosphinoyl)-1, 4-benzenediol
  • Environment-friendly preparation method of phosphorus flame retardant, namely 2-(diphenylphosphinoyl)-1, 4-benzenediol
  • Environment-friendly preparation method of phosphorus flame retardant, namely 2-(diphenylphosphinoyl)-1, 4-benzenediol

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Effect test

Embodiment 1

[0021] Equipped with mechanical stirring, thermometer, reflux condenser, N 2 In the 250ml dry four-necked flask of the catheter, feed dry nitrogen to remove the air in the flask, then add 22.0g (0.1mol) diphenylphosphine oxide, drop 1.8g (0.1mol) water at room temperature, and react at room temperature for 1 hour , then slowly add 50g of absolute ethanol and 10.8g (0.1mol) of p-benzoquinone mixture, react at room temperature for 2 hours, filter to obtain light yellow solid powder, then wash with 50g of absolute ethanol under reflux for 0.5 hour, cool Filter to obtain white solid powder, i.e. the product 2-(diphenylphosphono)-1,4-benzenediol, the yield is 81%, the infrared spectrum and NMR spectrum of the product are shown in figure 1 and figure 2 ;

Embodiment 2

[0023] Embodiment 2 has changed the proportioning of diphenylphosphine chloride and water, and concrete synthetic technique is as follows:

[0024] Equipped with mechanical stirring, thermometer, reflux condenser, N 2 In the 250ml dry four-necked flask of the catheter, feed dry nitrogen to remove the air in the flask, then add 22.0g (0.1mol) diphenylphosphine oxide, add 2.7g (0.15mol) water dropwise at room temperature, and react at room temperature for 1 hour , and then slowly add 50g of absolute ethanol and 10.8g (0.1mol) of p-benzoquinone mixture, react at room temperature for 2 hours, filter to obtain light yellow solid powder, then wash 0.5 pieces with 50g of absolute ethanol under reflux hours, cooled, filtered, and dried to obtain a white solid powder, the product 2-(diphenylphosphono)-1,4-benzenediol, with a yield of 94%.

Embodiment 3

[0026] Embodiment 3 has changed the proportioning of diphenylphosphine chloride and water, and concrete synthetic technique is as follows:

[0027] Equipped with mechanical stirring, thermometer, reflux condenser, N 2 In the 250ml dry four-necked flask of the catheter, feed dry nitrogen to remove the air in the flask, then add 22.0g (0.1mol) diphenylphosphine oxide, add 3.6g (0.2mol) water dropwise at room temperature, and react at room temperature for 1 hour , and then slowly add 50g of absolute ethanol and 10.8g (0.1mol) of p-benzoquinone mixture, react at room temperature for 2 hours, filter to obtain light yellow solid powder, then wash 0.5 pieces with 50g of absolute ethanol under reflux hours, cooled, filtered, and dried to obtain a white solid powder, the product 2-(diphenylphosphono)-1,4-benzenediol, with a yield of 95%.

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Abstract

The invention discloses an environment-friendly preparation method of a phosphorus flame retardant, namely 2-(diphenylphosphinoyl)-1, 4-benzenediol. Chlorodiphenylphosphine is taken as a reaction raw material, a one-pot method is adopted for skipping the purification process of the chlorodiphenylphosphine and further directly synthesizing the 2-(diphenylphosphinoyl)-1, 4-benzenediol, and a solvent and a purification solvent, which are used by the environment-friendly preparation method are alcohols, so that the environment-friendly preparation method has the advantages of low toxicity, high yield of above 90%, capability of greatly reducing production cost and effect of meeting environment-friendly and high-efficient requirements.

Description

technical field [0001] The invention relates to the field of polymer materials, in particular to an environmentally friendly and efficient preparation method of phosphorus-based flame retardants. Background technique [0002] 9,10-dihydro-9-oxo-10-phosphaphenanthrene-10-oxide (DOPO) reactive flame retardant is an important flame retardant, which can be cured by epoxy resin prepolymer To obtain a certain flame retardant grade of epoxy resin cured product, Wang et al. (Synthesis and properties of epoxy resins containing2-(6-oxid-6H-dibenz(c,e)(1,2)oxaphosphorin-6-yl)1,4 -benzonediol[J], Polym,1998,39(23):5819–5826.) The addition reaction of DOPO to benzoquinone is used for the curing of bisphenol A epoxy resin. When the mass fraction of phosphorus is 2.1%, the ring The UL94 test of the epoxy resin cured product reaches the V-0 level. However, due to the high price of DOPO, such a high amount of addition limits its practical application, and a large amount of addition will al...

Claims

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Application Information

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IPC IPC(8): C07F9/53C08K5/5397
Inventor 王忠卫侯计金伍清浴
Owner QINGDAO FUSILIN CHEM SCI & TECH
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