DOPO derivatives as well as flame retardant and flame-retardant material containing same

一种阻燃高分子、高分子材料的技术，应用在一类DOPO衍生物及包含其的阻燃剂和阻燃材料领域，能够解决高分子材料提早降解、降低阻燃剂热稳定性、增加被氧化性能等问题

Inactive Publication Date: 2017-05-31
NINGBO INST OF MATERIALS TECH & ENG CHINESE ACAD OF SCI +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The introduction of hydroxyl groups reduces the thermal stability of flame retardants, which is unfavorable to the processing of engineering plastics
The introduction of alkoxy group increases the oxidized performance, which will lead to the early degradation of polymer materials
[0010] One object of the present invention is to provide a kind of halogen-free flame retardant based on DOPO compound, this halogen-free flame retardant not only has good flame retardant effect, but also has very high thermal stability and chemical stability, can overcome existing DiDOPO Disadvantages of insufficient chemical resistance and strong plasticity

Method used

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  • DOPO derivatives as well as flame retardant and flame-retardant material containing same
  • DOPO derivatives as well as flame retardant and flame-retardant material containing same
  • DOPO derivatives as well as flame retardant and flame-retardant material containing same

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0083] Embodiment 1 has the preparation of formula (2) structure compound

[0084] DOPO (86.40 g, 0.40 mol), acetophenone (24.05 g, 0.20 mol) and 10 ml of xylene were added to a three-necked flask equipped with a thermometer, a water separator, a magnetic stir bar and a constant pressure funnel. Under nitrogen protection, the mixture was heated to 154°C, and phosphorus oxychloride was added dropwise. POCl 3 (30.25g) was slowly added dropwise to the reaction solution within 25 hours, and the distillate was collected in the water trap, keeping the reaction temperature at 154-160°C. After dropping phosphorus oxychloride, keep warm for half an hour. After cooling, add 120g of isopropanol, stir under reflux, most of the crude product dissolves after softening, and the system becomes turbid. Stirring was stopped, cooled, and a large amount of product precipitated after standing for a period of time. Suction filtration, the solid product was first washed with a small amount of is...

Embodiment 2

[0086] Embodiment 2 has the preparation of formula (3) structure compound

[0087] DOPO (86.40 g, 0.40 mol) and naphthalene ethyl ketone (34.04 g, 0.20 mol) were added into a three-necked flask equipped with a thermometer, a magnetic stir bar and a constant pressure funnel. Under nitrogen protection, the mixture was heated to 170°C, and phosphorus oxychloride was added dropwise. POCl 3 (15.96g) was slowly added dropwise in the reaction solution within 20 hours, keeping the reaction temperature at 170-180 degrees. After dropping phosphorus oxychloride, keep warm for half an hour. 31 P NMR spectrum showed no starting material. Cool, add 50ml of 90% ethanol to dissolve, then drop about 60ml of 2.5% Na 2 CO 3 Solution The pH of the reaction solution was adjusted to 6-7, and the white solid product was obtained by suction filtration after reflux for half an hour. Yield 70.6%.

[0088] The obtained product is characterized by H spectrum and P spectrum on a magnetic resonance ...

Embodiment 3

[0090] According to the preparation method in Example 1, phosphorus oxychloride was changed into 13.7 grams of phosphorus trichloride to obtain a compound having the structure of formula (2). Yield 75.8%.

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PUM

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Abstract

The invention relates to compounds capable of being taken as novel halogen-free flame retardants. The compounds are prepared from aryl ketones and DOPO compounds under the action of an acid catalyst. The compounds have good flame retardant effect, thermal stability and chemical stability.

Description

[0001] The present invention is a divisional case of a patent application with an application date of July 14, 2014, an application number of 201410333261.5, and a patent application titled "A Class of DOPO Derivatives, Its Preparation Method and Application". technical field [0002] The application relates to a halogen-free flame retardant and a preparation process thereof. Background technique [0003] Polymer materials are widely used in electronic appliances, automobiles, construction, textiles and other industries. However, due to the flammability of polymer materials, it is necessary to add flame retardants in actual use to meet the requirements of fire safety. Traditionally, brominated flame retardants are usually added to polymer materials to achieve flame retardant effects. However, when brominated flame retardants burn, they will produce strong irritating hydrogen bromide gas, thick smoke, and even some strong carcinogenic substances, which limits the use of brom...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08K5/5313C08K5/134C08K5/315C08K7/14C08L69/00C08L63/00C07F9/6574
Inventor 姚强周浩张伟伟曹微虹刘正西徐子平
Owner NINGBO INST OF MATERIALS TECH & ENG CHINESE ACAD OF SCI
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