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Preparation method of high-purity DOPO (9,10-dihydro-9-oxa-10- phosphaphenanthrene-10-oxide) derivative

A derivative and high-purity technology, applied in the field of flame retardants, can solve problems affecting applications and achieve short reaction routes

Active Publication Date: 2013-11-27
JIANGSU YOKE TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The patent uses DOPO and ethylene glycol (EG) as raw materials to synthesize the DOPO derivatives, and the resulting product is a mixture of three isomers (enantiomers) of compound I, of which compound I (RS type) The melting point is the highest, due to the existence of two other low-melting point isomers (RR and SS types), the melting point of the product is only about 250 degrees, which affects its application in some special fields; The method for converting melting point isomers to high melting point isomers, the resulting product is still a mixture, but the content of compound I has increased to varying degrees

Method used

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  • Preparation method of high-purity DOPO (9,10-dihydro-9-oxa-10- phosphaphenanthrene-10-oxide) derivative

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Experimental program
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Effect test

Embodiment 1

[0017] Embodiment 1, the preparation of DOPO derivative compound I (add catalyst I)

[0018] Add CDOP (47 g, 0.20 mol), triethylamine (20.24 g, 0.20 mol), sodium iodide (1.50 g) and 100 ml xylene to the flask, and slowly add ethylene glycol (4.97 g , 0.08 mol), keep the temperature of the system not exceeding 20 degrees during the dropwise addition, react at about 20 degrees for 2 hours after the addition, and then raise the temperature to 120 degrees for 3 hours. After cooling, filter, add 100mL of ethanol to the filtrate, stir at 80°C for half an hour, then filter while hot to obtain 30.4g of the product, with a yield of 83%. (Because excess CDOP can be recycled, the yield is calculated based on ethylene glycol).

Embodiment 2

[0019] Embodiment 2, preparation of DOPO derivative compound I (without catalyst I)

[0020] Add CDOP (70.4 g, 0.30 mol), iodine (2.0 g) and 80 ml of diphenylmethane into the flask, heat to 160 degrees, then slowly add ethylene glycol (9.31 g, 0.15 mol) to it, after adding The reaction was continued at temperature for 20 hours. Cool to about 80 degrees, add 90mL of ethanol to the system, stir for half an hour, and filter while hot to obtain 55.1g of the product, with a yield of 80%.

Embodiment 3-19

[0021] Embodiment 3-19, with reference to Embodiment 1 and 2, modify some parameters, as shown in the following table:

[0022]

[0023] In this table, as in Example 3, the reaction temperature is 10 / 120, and the reaction time is 3 / 12, which means that the temperature of the system should not exceed 10 degrees during the dropwise addition of ethylene glycol, and react at about 10 degrees for 3 hours after the addition , and then warming up to 120 degrees for 12 hours, the other embodiments are the same.

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Abstract

The invention provides a preparation method of a high-purity DOPO (9,10-dihydro-9-oxa-10- phosphaphenanthrene-10-oxide) derivative, and relates to a flame retardant in the field of chemical materials. According to the preparation method, CDOP (10-chloro-9,10-dihydro-9-oxa-10-phosphaphenanthrene) is used as a raw material and reacts with ethylene glycol under the action of a catalyst, wherein the reaction temperature is 10-200 DEG C, and the reaction time is 5 to 30 hours, so that a product with high optical purity can be directly obtained. The preparation method has the advantages that reaction routes are short, the product does not contain another two isomers, and the melting point of the product reaches up to about 300 DEG C. The high-purity DOPO derivative can be used as the flame retardant.

Description

technical field [0001] The invention relates to a flame retardant in the field of chemical materials, in particular to a preparation method of a high-purity DOPO (9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide) derivative. Background technique [0002] Epoxy resins are widely used in various electronic components, electrical equipment, automotive parts, and sports facilities due to their special properties such as adhesion, heat resistance, and moldability. At present, brominated flame retardants account for a large proportion of epoxy resins related to the electrical and electronic fields, such as copper clad laminates and printed circuit boards. However, based on the consideration that halogens can cause harm to the environment and human safety, the more environmentally friendly phosphorus-based flame retardants have gradually received attention. In the field of epoxy resin sheets, the application of additive phosphorus flame retardants is relatively rare, because it ...

Claims

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Application Information

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IPC IPC(8): C07F9/6574
Inventor 沈琦陈杜刚吴俊东刘明霞
Owner JIANGSU YOKE TECH
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