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Polyborazine ceramic precursor and preparation method thereof

A technology of ceramic precursors and polyborazane, which is applied in the field of polyborazane ceramic precursors and its preparation, can solve the problems of low boron content, difficulty in exerting the excellent performance of boron atoms, low activity, etc., and achieve simple preparation equipment , High utilization rate, rich source of monomer

Inactive Publication Date: 2012-01-18
XI AN JIAOTONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Especially in resin-based composite materials, ordinary boron-containing compounds have low activity, and the boron-containing materials prepared from them have low boron content, and it is difficult to exert the excellent performance of boron atoms.

Method used

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  • Polyborazine ceramic precursor and preparation method thereof
  • Polyborazine ceramic precursor and preparation method thereof
  • Polyborazine ceramic precursor and preparation method thereof

Examples

Experimental program
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Effect test

example 1

[0018] Example 1: 0.1 mole of 1,3 propylenediamine in 100 mL of DMF was added to a 250 mL three-neck flask under nitrogen protection, and 0.06 mole of boron trifluoride in ether was slowly added thereto under stirring at -10°C. After the dropwise addition, the system was reacted at 0° C. for 10 h, then heated to 60° C. and reacted at this temperature for 4 h. Then react at 150°C for 24h. After the reaction, the solvent was distilled off under reduced pressure. The obtained substance was dissolved-precipitated three times with ethanol-anhydrous ether, and vacuum-dried at 60° C. for 24 hours to obtain the target polymer as a pale yellow solid with a yield of 65%.

example 2

[0019] Example 2: Add 0.15 moles of p-phenylenediamine in 100 mL of sulfolane solution into a 250 mL three-neck flask under nitrogen protection, and slowly add 0.05 moles of boron trifluoride in ether to it under stirring at 0°C. After the dropwise addition, the system was reacted at 5°C for 6h, then heated to 80°C and reacted at this temperature for 4h. Then react at 120°C for 12h and at 200°C for 8h. After the reaction, the solvent was distilled off under reduced pressure. The obtained substance was dissolved-precipitated three times with ethanol-anhydrous ether, and vacuum-dried at 60° C. for 24 hours to obtain the target polymer as a pale yellow solid with a yield of 78%.

example 3

[0020] Example 3: Under nitrogen protection, 0.20 moles of p-phenylenediamine in 100 mL of dimethyl sulfoxide solution was added to a 250 mL three-necked flask, and 0.05 moles of boron trichloride in toluene was slowly added thereto under stirring at -10°C solution. After the dropwise addition, the system was reacted at 5°C for 2h, then heated to 80°C and reacted at this temperature for 4h. Then react at 120°C for 12h and at 160°C for 24h. After the reaction, the solvent was distilled off under reduced pressure. The resulting substance was precipitated three times with ethanol-anhydrous ether, and dried under vacuum at 60° C. for 24 hours to obtain the target polymer as a pale yellow solid with a yield of 81%.

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Abstract

The invention relates to a polyborazine ceramic precursor and a preparation method thereof. According to the invention, a solution polycondensation method is used and the preparation method comprises the following steps of: using boron-containing alkylogen and diamine as monomers; adding the boron-containing alkylogen and diamine into an organic solvent under an inert gas or nitrogen protection; and obtaining the precursor through a stepwise heating polycondensation at a temperature of -20-300 DEG C. According to the invention, polyborazine is white solid and has an excellent solubility in ethanol, acetone and other commonly used solvents; the skeletal structure of the precursor has a large number of active terminal groups so that the precursor can participate in curing processes of an epoxy resin and a benzoxazine resin, can be used for preparing the ceramic precursor and a high-performance composite material; and particularly, the polymer has higher oxidation-resistant and heat-resistant performance and a potential application prospect in ablation protection materials.

Description

technical field [0001] The invention relates to a ceramic precursor, its preparation method and its potential application in resin-based ablation-resistant materials. Background technique [0002] High-performance ceramic materials have excellent heat resistance and oxidation resistance, and have important applications in the field of ablative materials. However, ceramic materials have a high melting point and poor processability. The precursor pyrolysis conversion ceramic process has the characteristics of excellent organic polymer molding, and also has the properties of molecular design, good processability and low-temperature ceramicization. Therefore, the precursor polymer-to-ceramic conversion process has a wide range of applications in the fields of adhesives, coatings, and membrane materials. [0003] Compounds containing boron atoms tend to form diboron trioxide in an oxidizing environment. At high temperature, the diboron trioxide layer of glassy structure can in...

Claims

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Application Information

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IPC IPC(8): C08G79/08C04B35/58C08L79/04C08K3/38
Inventor 刘育红井新利杨鑫王彪
Owner XI AN JIAOTONG UNIV
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