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Phosphor silicon nitrogen ternary coordination fire retardant, preparation method and application

A flame retardant material, vinyl silazane technology, applied in the field of functional flame retardants, can solve the problems of complex preparation process, no batch products, and supply, etc., and achieve the effect of excellent flame retardant performance

Active Publication Date: 2013-05-01
INST OF CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the phosphorus-silicon-nitrogen ternary synergistic flame retardant has a good flame retardant effect on polymer materials, due to its complicated preparation process, there is currently no batch product available on the market.

Method used

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  • Phosphor silicon nitrogen ternary coordination fire retardant, preparation method and application
  • Phosphor silicon nitrogen ternary coordination fire retardant, preparation method and application
  • Phosphor silicon nitrogen ternary coordination fire retardant, preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] In a reactor equipped with nitrogen inlet, condenser and thermometer, 4.04g (0.02mol) of diphenylphosphine oxide (DPPO) and 1.85g (0.01mol) of 1,1,3,3-tetramethyl- Add 1,3-divinyldisilazane to 10ml of acetone in turn, stir at 15°C until clear and transparent, under the protection of nitrogen, control the temperature at 15°C, add 4ml of 0.5M tripropyl Boron tetrahydrofuran solution; after the dropwise addition, the addition reaction was stopped at 15°C for 1 hour, the solvent was evaporated, washed with water several times, and dried to obtain 5.08 g of white solid (Compound 1), with a yield of 86%.

[0040] The structural detection data of this compound are as follows (the NMR spectrum, NMR carbon spectrum, NMR phosphorus spectrum, NMR silicon spectrum, mass spectrum (MALDI-TOF) figure, infrared spectrum and DSC spectrum of this compound are respectively as follows figure 1 , figure 2 , image 3 , Figure 4 Figure 5 , Figure 6 and Figure 7 shown.

[0041] Mel...

Embodiment 2

[0051] In a reactor equipped with nitrogen inlet, condenser and thermometer, 41.4g (0.205mol) of diphenylphosphine oxide (DPPO) and 18.5g (0.1mol) of 1,1,3,3-tetramethyl- Add 1,3-divinyldisilazane to 100ml of acetone in turn, stir at 15°C until clear and transparent, under nitrogen protection, control the temperature at 15°C, add 40ml of 0.5M tripropyl Boron tetrahydrofuran solution; after the dropwise addition, the addition reaction was stopped at 15°C for 10 hours, the solvent was evaporated, washed with water several times, and dried to obtain 53.7 g of white solid (compound 2), with a yield of 88%.

[0052] The structural detection data of this compound are as follows (the NMR spectrum, NMR carbon spectrum, NMR phosphorus spectrum, NMR silicon spectrum, mass spectrum (MALDI-TOF) figure, infrared spectrum and DSC spectrum of this compound are respectively as follows figure 1 , figure 2 , image 3 , Figure 4 Figure 5 , Figure 6 and Figure 7 shown.

[0053] Meltin...

Embodiment 3

[0062] In a reactor equipped with nitrogen inlet, condenser and thermometer, 4.04g (0.02mol) of diphenylphosphine oxide (DPPO) and 1.85g (0.01mol) of 1,1,3,3-tetramethyl- Add 1,3-divinyldisilazane to 10ml of tetrahydrofuran in turn, stir at 15°C until clear and transparent, under nitrogen protection, control the temperature at 15°C, add 5ml of tributyl tributyl with a concentration of 0.5M dropwise within 0.5 hours Boron n-hexane solution; after the dropwise addition, the addition reaction was stopped at 15°C for 2 hours, the solvent was evaporated, washed with water several times, and dried to obtain 4.95 g of white solid (compound 3), with a yield of 84%.

[0063] The structural detection data of this compound are as follows (the NMR spectrum, NMR carbon spectrum, NMR phosphorus spectrum, NMR silicon spectrum, mass spectrum (MALDI-TOF) figure, infrared spectrum and DSC spectrum of this compound are respectively as follows figure 1 , figure 2 , image 3 , Figure 4 Figu...

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Abstract

The invention discloses a phosphor silicon nitrogen ternary coordination fire retardant, a preparation method and an application. A structural general formula of the phosphor silicon nitrogen ternary coordination fire retardant is shown as a as formula I. According to the invention, an organic boron catalyst is used, diphenylphosphine oxide and its derivative are used for generating an addition reaction with silicon nitrogen alkane containing a carbon-carbon double bond to prepare a novel phosphor, silicon and nitrogen-containing compound. The compound has the characteristics of hydrolysis resistance and easy purification and the like. According to the invention, the phosphor element, the silicon element and the nitrogen element in a molecular structure of the compound can be individually performed a flame retardation effect, and simultaneously performed synergism, thereby the excellent flame retardation performance is provided on the general polymeric materials.

Description

technical field [0001] The invention belongs to the field of functional flame retardants, and relates to a phosphorus-silicon-nitrogen ternary synergistic flame retardant and its preparation method and application. Background technique [0002] In the past few decades, polymers have been widely used due to their excellent properties. However, due to the flammability of common polymer materials, fires are often induced, so they usually need to be used together with flame retardants. Adding flame retardants to the polymer body is the most effective means to improve the flame retardancy of polymer materials. [0003] While exploring and synthesizing new high-efficiency flame retardants, people also use different flame retardants together to reduce the amount of flame retardants and improve the flame retardant efficiency. In the process of using different flame retardants together, due to the synergistic effect of the flame retardant mechanism of different flame retardants, th...

Claims

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Application Information

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IPC IPC(8): C07F9/53C08L63/04C08L61/06C08L23/06C08L69/00C08L67/02C08L77/00C08K5/5445
Inventor 杨士勇李志生刘金刚沈登雄
Owner INST OF CHEM CHINESE ACAD OF SCI
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