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Flame retardant containing phosphonitrile-DOPO structure and preparation method of flame retardant agent

A technology of flame retardant and cyclotriphosphazene, which is applied in the field of flame retardant containing phosphazene-DOPO structure and its preparation, to achieve the effects of improved flame retardant performance, increased flame retardant efficiency, and simple preparation process

Inactive Publication Date: 2019-03-01
CHINA BLUESTAR CHENGRAND CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At the same time, the high heat-resistant phosphazene structure endows the flame retardant with good heat resistance and meets the requirements of high-temperature processing conditions. By combining biorenewable vanillin as a lap block with DOPO, the flame retardant performance is improved. At the same time, it also solves the problem of some adverse effects of the single DOPO flame retardant on the performance of the epoxy resin material itself with the increase of the addition amount, and the compatibility with the epoxy resin material is good, and the flame retardant The preparation process is simple, the yield is as high as more than 80%, it is easy to realize industrial production, and it is green and environmentally friendly

Method used

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  • Flame retardant containing phosphonitrile-DOPO structure and preparation method of flame retardant agent
  • Flame retardant containing phosphonitrile-DOPO structure and preparation method of flame retardant agent
  • Flame retardant containing phosphonitrile-DOPO structure and preparation method of flame retardant agent

Examples

Experimental program
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Effect test

Embodiment 1

[0035] Example 1 A flame retardant containing a phosphazene-DOPO structure, its structural formula is as follows:

[0036] .

Embodiment 2

[0037] The preparation of embodiment 2 intermediate product I

[0038] Add 7.9g of vanillin and 3g of cyclotriphosphazene to 109g of dioxane, heat the reaction at 80°C for 8h, remove the solvent, wash and dry to obtain 8.1g of intermediate product I, with a yield of 90%.

[0039] Its infrared (FTIR) test results are as follows:

[0040] FTIR (KBr): P-Cl bond characteristic absorption peak disappears at 525cm-1; benzene ring and aldehyde carbonyl strongly absorb at 1593cm-1 and 1676.5cm-1 respectively; phosphazene structural features appear at 1225cm-1 and 868cm-1 absorb. It shows that vanillin reacts with cyclotriphosphazene to generate the target intermediate product.

Embodiment 3

[0041] Example 3 Preparation of flame retardant containing phosphazene-DOPO structure

[0042] (1) Add 15.8g of vanillin and 6g of cyclotriphosphazene to 218g of dioxane, heat and react at 80°C for 8h, and obtain a reaction system containing intermediate product I;

[0043] (2) Add 22.5g of DOPO into the reaction system obtained in step (1), stir and heat at 80°C for 8 hours, remove dioxane after the reaction, wash and dry to obtain a light yellow flame-retardant compound containing phosphazene-DOPO structure Agent 34.5g, productive rate is 85%.

[0044] Infrared (FTIR) of the flame retardant prepared in this example is as follows: figure 1 As shown, the analysis results are as follows:

[0045] FTIR (KBr): The aldehyde carbonyl group disappears at a wave number of 1676.5cm-1, and -OH absorption appears at a wave number of 3398cm-1; the absorption peak at a wave number of 1232cm-1 is P=O, and 931.5cm-1 and 756.5cm-1 are P-O -Ph absorption, 870cm-1, 1225cm-1 is P=N structure a...

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Abstract

The invention relates to the technical field of flame retardants and particularly discloses a flame retardant containing a phosphonitrile-DOPO structure and a preparation method of the flame retardantagent. The preparation method comprises the following steps: firstly, adding cyclotriphosphazene and vanillin into an organic solvent, and carrying out heating reaction at 60 to 80 DEG C for 6 to 8 hours to obtain a reaction system containing an intermediate product; secondly, adding DOPO into the reaction system obtained in the first step, and carrying out stirring and heating reaction at 60 to80 DEG C for 6 to 8 hours; after the reaction is ended, removing a solvent, washing and drying to obtain the flame retardant containing the phosphonitrile-DOPO structure. The flame retardant integrates phosphorus and nitrogen flame retardant elements, and has the advantages of a good flame retardant synergistic effect and heat resistance, remarkably-improved flame retardant efficiency along with the increase of additive amount, good compatibility with epoxy resin, easiness in realization of industrial production, greenness and environmental protection; the flame retardant belongs to an efficient low-toxicity, halogen-free and environment-friendly flame retardant.

Description

technical field [0001] The invention relates to the technical field of flame retardant synthesis, in particular, the invention relates to a flame retardant containing a phosphazene-DOPO structure and a preparation method thereof. Background technique [0002] Cyclotriphosphazene is a new type of phosphorus-containing flame retardant framework material. Its stable six-membered ring structure can provide high heat resistance. At the same time, its highly active P-Cl bond has rich derivatization properties, so it can be prepared into various A variety of derivatives, because the derivatives can have both organic and inorganic properties, so they have excellent thermal stability, corrosion resistance, water resistance, chemical resistance, good compatibility with materials, and have a great influence on material properties At the same time, it has been widely studied in the field of flame retardancy and has broad application prospects. [0003] 9,10-dihydro-9-oxa-10-phosphaphen...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/6593C08K5/5399C08L63/00
CPCC07F9/65815C08K5/5399C08L2201/02C08L2201/08C08L63/00
Inventor 邓清田唐培徐亭宋升吴勇
Owner CHINA BLUESTAR CHENGRAND CO LTD
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