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Halogen-free DOPO (9,10-dihydro-9-oxa-10-phosphaphenanthrene 10-oxide)-based hyperbranched structure phosphate flame retardant and preparation method thereof

A phosphoric acid ester and flame retardant technology, applied in the field of DOPO-based hyperbranched structure phosphoric acid ester halogen-free flame retardant and its preparation, can solve the problems of poor compatibility, low phosphorus content of hyperbranched phosphorus-containing flame retardant and the like , to achieve the effects of good compatibility, easy control of reaction conditions and high flame retardant efficiency

Inactive Publication Date: 2017-12-22
BEIJING INSTITUTE OF TECHNOLOGYGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The purpose of the present invention is to provide a DOPO-based hyperbranched structure phosphate halogen-free Flame retardant and preparation method thereof

Method used

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  • Halogen-free DOPO (9,10-dihydro-9-oxa-10-phosphaphenanthrene 10-oxide)-based hyperbranched structure phosphate flame retardant and preparation method thereof
  • Halogen-free DOPO (9,10-dihydro-9-oxa-10-phosphaphenanthrene 10-oxide)-based hyperbranched structure phosphate flame retardant and preparation method thereof
  • Halogen-free DOPO (9,10-dihydro-9-oxa-10-phosphaphenanthrene 10-oxide)-based hyperbranched structure phosphate flame retardant and preparation method thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] A DOPO-based hyperbranched structure phosphate halogen-free flame retardant, its general structure is as follows:

[0035]

[0036] Where R is the following structure:

[0037]

[0038] A preparation method of DOPO-based hyperbranched structure phosphate ester halogen-free flame retardant, the specific steps are as follows:

[0039] (1) Synthesis of intermediate DOPO-phOH

[0040] Measure 21.40g (0.10mol) of 4,4'-dihydroxybenzophenone, 47.52g (0.22mol) of DOPO and 350mL of anhydrous toluene solvent, and add them to the inlet and outlet with thermometer, stirrer, condenser and protective gas In a 500mL reaction vessel, under the condition of nitrogen gas, the reaction was carried out at 80°C for 2 hours, and then at 110°C for 2 hours. The obtained precipitate was suction filtered while hot, washed twice with anhydrous toluene, and dried in a vacuum oven at 100° C. for 2 hours to obtain 52.45 g of a white powdery solid product with a yield of 81.2%.

[0041] (2) Synthesis of DOPO...

Embodiment 2

[0048] A DOPO-based hyperbranched structure phosphate halogen-free flame retardant, its general structure is as follows:

[0049]

[0050] Where R is the following structure:

[0051]

[0052] A preparation method of DOPO-based hyperbranched structure phosphate ester halogen-free flame retardant, the specific steps are as follows:

[0053] (1) Synthesis of intermediate DOPO-TPA

[0054] Measure 13.13g (0.10mol) of terephthalaldehyde, 45.36g (0.21mol) of DOPO and 300mL of anhydrous benzene solvent, and add them to a 500mL reaction vessel with thermometer, stirrer, condenser, and protective gas inlet and outlet. Under the condition of nitrogen gas, the reaction was carried out at 70°C for 4 hours and then at 80°C for 1 hour. The obtained precipitate was suction filtered while hot, washed once with anhydrous benzene, and dried in a vacuum oven at 70° C. for 3 hours to obtain 50.05 g of a white powdery solid product with a yield of 88.9%.

[0055] (2) Synthesis of DOPO-based hyperbranched...

Embodiment 3

[0059] A DOPO-based hyperbranched structure phosphate halogen-free flame retardant, its general structure is as follows:

[0060]

[0061] Where R is the following structure:

[0062]

[0063] A preparation method of DOPO-based hyperbranched structure phosphate ester halogen-free flame retardant, the specific steps are as follows:

[0064] (1) Synthesis of intermediate DOPO-PHBA

[0065] Measure 12.21g (0.10mol) of p-hydroxybenzaldehyde, 45.36g (0.21mol) of DOPO and 200mL of anhydrous toluene solvent, add them to a 500mL reaction vessel with thermometer, stirrer, condenser and protective gas inlet and outlet. Under the condition of nitrogen gas, after reacting at 100°C for 1 hour, react at 110°C for 2 hours. The obtained precipitate was suction filtered while hot, washed twice with anhydrous toluene, and dried in a vacuum oven at 100° C. for 4 hours to obtain 44.04 g of a white granular solid product with a yield of 79.5%.

[0066] (2) Synthesis of DOPO-based hyperbranched structure p...

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Abstract

The invention relates to a halogen-free DOPO (9,10-dihydro-9-oxa-10-phosphaphenanthrene 10-oxide)-based hyperbranched structure phosphate flame retardant and a preparation method thereof and belongs to the technical field of phosphorus-containing flame retardants. According to the method, the hyperbranched structure phosphate flame retardant with high phosphorus content is prepared from two phosphorus-containing monomers, namely, a DOPO-based intermediate and phosphorus oxychloride serving as reaction units, and the purpose of increasing the phosphorus content of the flame retardant is achieved while the macromolecular flame retardant is obtained. The defects of poor compatibility of a micromolecular phosphorus-containing flame retardant and low phosphorus content of conventional hyperbranched flame retardants are effectively overcome. The synthesized flame retardant has the advantages of high phosphorus content, high molecular weight, high combustion efficiency, good compatibility with a flame-retardant substrate, low probability of migration and the like.

Description

Technical field [0001] The invention relates to a DOPO-based hyperbranched structure phosphate ester halogen-free flame retardant and a preparation method thereof, and belongs to the technical field of phosphorus-containing flame retardants. Background technique [0002] Polymer materials have the advantages of low density, high specific strength, high toughness and good fatigue resistance. They are widely used in packaging, construction, and machinery industry. However, polymer materials are mostly composed of C, H, and O elements, which leads to the widespread flammability of polymer materials. In recent years, fires caused by polymer materials have occurred frequently, posing a serious threat to people's lives and property, so it is very important to treat them with flame retardant. [0003] In the past ten years, flame-retardant modification of flammable polymer materials has always been a hot spot in the research of polymer composite materials. Various types of flame retardan...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G83/00C08G79/04C08L23/12C08L87/00C08L85/02
CPCC08G79/04C08G83/005C08L23/12C08L2201/02C08L2201/22C08L87/00C08L85/02
Inventor 李树磊王银杰
Owner BEIJING INSTITUTE OF TECHNOLOGYGY
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