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Multi-reaction functionality phosphaphenanthrene/siloxane double base macromolecule flame retardant and preparation method thereof

A technology of reactive functions and phosphaphenanthrene, which is applied in the field of multi-reactive functional double-base macromolecules and its preparation, can solve the problems that phosphaphenanthrene/siloxane double-base macromolecules have not been reported, and achieve excellent thermal stability , high yield, simple and easy preparation process

Active Publication Date: 2021-09-17
BEIJING TECHNOLOGY AND BUSINESS UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In order to explore more efficient phosphaphenanthrene / siloxane double-base macromolecular flame retardants, the present invention designed and prepared two kinds of multi-reaction functional phosphaphenanthrene / siloxane double-base macromolecule with different group ratios and construction forms. Molecules; the multi-reactive functional phosphaphenanthrene / siloxane diradical macromolecules announced by the present invention have not been reported in the literature and published materials

Method used

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  • Multi-reaction functionality phosphaphenanthrene/siloxane double base macromolecule flame retardant and preparation method thereof
  • Multi-reaction functionality phosphaphenanthrene/siloxane double base macromolecule flame retardant and preparation method thereof
  • Multi-reaction functionality phosphaphenanthrene/siloxane double base macromolecule flame retardant and preparation method thereof

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Experimental program
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Embodiment 1

[0019] Under stirring condition, DDBA (44.45g, 0.060mol) was dissolved in the dichloroethane (350mL) that pre-dehydrated, after DDBA dissolved completely, slowly added phenyltrichlorosilane (3.81g, 0.018mol), After stirring the reaction for 20 hours at 85°C, the reaction was terminated, and the residual DDBA in the TriDSi was removed by solvent washing to obtain the target product TriDSi, with a yield of 98.5%, a purity of 99.5%, and a temperature of 1wt.% for weight loss. 374°C.

Embodiment 2

[0021] Under stirring condition, DDBA (133.34g, 0.180mol) was dissolved in the chlorobenzene (1500mL) that dehydrated beforehand, after DDBA dissolved completely, slowly added phenyl trichlorosilane (8.46g, 0.040mol), at 135 After reflux reaction at ℃ for 18 hours, the reaction was terminated, and the residual DDBA in TriDSi was removed by solvent washing to obtain the target product TriDSi, with a yield of 99.0%, a purity of 99.2%, and a weight loss of 1wt.%. The temperature was 372°C .

Embodiment 3

[0023] Under the condition of stirring, DDBA (44.45g, 0.060mol) was dissolved in tetrahydrofuran (300mL) which was pre-dehydrated and dried. After DDBA was completely dissolved, phenyltrichlorosilane (2.12g, 0.010mol) was slowly added, and After stirring the reaction for 15 hours at ℃, the reaction was terminated, and the residual DDBA in TriDSi was removed by solvent washing to obtain the target product TriDSi, with a yield of 98.2%, a purity of 99.3%, and a weight loss of 1wt.%. The temperature was 375°C .

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Abstract

The invention discloses a multi-reaction functionality phosphaphenanthrene / siloxane double-base macromolecular flame retardant and a preparation method thereof. The flame retardant is a three-reaction functionality double-base macromolecule TriDSi or a four-reaction functionality double base The macromolecular TetraDSi is prepared by condensation reaction of the phenolic hydroxyl group on bis(1-phosphaphenanthrene-propyl) bisphenol A with the silicon-chloride bond in phenyltrichlorosilane or tetrachlorosilane. The preparation process is simple and easy It is feasible and the yield is high; the multi-reaction functionality phosphaphenanthrene / siloxane double-base macromolecule TriDSi and TetraDSi announced by the present invention all have excellent thermal stability and efficient flame retardancy, and can efficiently improve epoxy resin, Polymer materials such as polycarbonate, polyamide, and polyurethane have flame retardant properties, and significantly improve the impact resistance of epoxy resin materials. They have very broad application prospects in high-end manufacturing and electronic appliances.

Description

technical field [0001] The invention relates to a multi-reactive functional diradical macromolecule based on phosphaphenanthrene and siloxane groups and a preparation method thereof, and belongs to the technical field of preparing flame retardants by chemical synthesis methods. Background technique [0002] In recent years, more and more flame-retardant groups have been extensively studied by researchers in the field of new high-efficiency flame-retardant compounds and polymer materials due to their unique flame-retardant effects and effective behavioral mechanisms, including phosphazenes, three Flame retardant groups such as oxazine, phosphaphenanthrene, silsesquioxane and borate; and 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO) The high reactivity and good flame retardant effect make the preparation of new high-efficiency phosphaphenanthrene derivative flame retardants from DOPO a research hotspot in the field of flame retardant in recent years. [0003] The ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/6574C08K5/5419C08K5/5415C08L63/00C08L69/00C08L77/00C08L75/04
CPCC07F9/657172C08K5/5415C08K5/5419C08L63/00C08L2201/02
Inventor 钱立军邱勇陈雅君许博
Owner BEIJING TECHNOLOGY AND BUSINESS UNIVERSITY