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Composition and preparation method thereof, flame retardant polymer material containing the composition

A flame retardant polymer and composition technology, applied in the field of flame retardants, can solve the problems of low melting point of double DOPO, inconvenient use, processing, etc.

Active Publication Date: 2020-06-09
NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] In order to solve the inconvenient use and processing problems caused by the low melting point of the above-mentioned pure double DOPO, the application provides a composition

Method used

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  • Composition and preparation method thereof, flame retardant polymer material containing the composition
  • Composition and preparation method thereof, flame retardant polymer material containing the composition
  • Composition and preparation method thereof, flame retardant polymer material containing the composition

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0110] Embodiment 1 has the preparation of the compound of structural formula 2 (c=0)

[0111] 51.06g (0.30mol) o-phenylphenol (abbreviated as OPP) and 0.41g zinc chloride are dropped into the 100ml there-necked flask equipped with constant pressure dropping funnel, Claisen tube, condenser tube, thermometer and magnetic stirring bar, Nitrogen. When the temperature in the system rises to 78°C and turns into a transparent liquid phase, start to add 45.33g of PCl dropwise 3 . During the dropwise addition, the reaction temperature was gradually increased to 165°C. PCl 3 After the dropwise addition was completed in 7.5 hours, the temperature was raised to 172° C. and kept warm until no HCl was generated. Then add 100g xylene to the system, and distill off excess PCl 3 . The crude product was obtained, and the product was denoted as DOPO-Cl. Take DOPO-Cl (33.41g, 142.5mmol) and 14ml of xylene into a three-necked flask equipped with a thermometer, a water separator, a magnetic...

Embodiment 2-15

[0112] Embodiment 2-15 has the preparation of the composition of structural formula 2 (c≠0)

[0113]The pure 6H-dibenzo[c,e[[1,2]oxaphosphorinane, 6,6'-(1,2-(1-phenyl)ethanediyl)bis -, 6,6'-dioxide and different organic compounds are mixed according to a certain ratio, and after stirring to make them fully mixed, the excess free solvent is evaporated at room temperature, and then dried in a vacuum oven at 150°C until the quality is constant . It was found that the obtained samples were all solid at 150°C, indicating that the melting point of these samples was higher than 150°C. Afterwards, the melting point of each sample was measured (referred to as melting point 1), and the content of organic compounds therein was determined by NMR (referred to as c1). After carrying out these tests, heat them to melting (the melting temperature is much higher than the boiling point of the organic compound), keep the heat for a certain period of time, until the organic compound is complete...

Embodiment 16

[0125] Preparation of embodiment 16 flame retardant polycarbonate

[0126] The American GE 141R PC polycarbonate plastic raw material (referred to as PC), Ciba antioxidant 1010 (the main chemical composition is tetrakis [3-(3,5-di-tert-butyl-4-hydroxyphenyl) propionic acid] quaternary Amyl alcohol ester), and the sample obtained from the above examples are mixed in plastic bags in advance according to the weight ratio of 94.75 / 0.25 / 5.0, and then extruded and granulated in a Brabender twin-screw extruder. The twin-screw extruder temperature was set at 270°C. Record whether the extrusion process is smooth or not, as shown in Table 2.

[0127] Table 2

[0128]

[0129] As can be seen from the table above, processing is smoother with the high melting point double DOPO (ie composition) containing the organic compound.

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Abstract

Disclosed is a composition, characterized in that the composition has a composition as represented by formula (1-1): B+cA formula (1-1), wherein B is selected from at least one compound of a chemical formula as represented by formula (1-2), A is selected from at least one of alcohols, amines, esters, ketones, ethers, nitriles, alkanes and cycloalkanes, and c is the ratio of A to B, and c = 0.0005-0.1. Also disclosed are a preparation method therefor and the use thereof.

Description

technical field [0001] The application relates to a composition composed of DOPO derivatives and organic compounds, its preparation process and application, and belongs to the field of flame retardants. Background technique [0002] Vinyl-containing compound prepared by reacting 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO) with dichloroethane, ethylene glycol or alkyl aryl ketone bridge chain (-CH 2 CH 2 -) or phenyl vinyl bridge (-CH(Ph)CH 2 -) DOPO derivatives, referred to as double DOPO, are known. [0003] Chinese patent application CN102428092A reports 6H-dibenzo[c,e[[1,2]oxaphosphorinane, 6,6'-(1,4-ethanediyl)bis-,6,6' -Dioxide and its preparation method [0004] Chinese patent CN104086593 reported 6H-dibenzo[c,e[[1,2]oxaphosphorinane, 6,6'-(1,2-(1-phenyl)ethanediyl)bis- , 6,6'-dioxygen compounds and methods for their preparation. [0005] Japanese patent application JPH11-106619 and Japanese patent application JP2001270993 reported double DOPOs wit...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08K5/5313C08K5/05C08L69/00C08L67/02
CPCC08K5/05C08K5/5313C08L2201/02C08L69/00C08L67/02
Inventor 姚强赵月英曹微虹唐天波
Owner NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI