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High-temperature resistant polyphosphazene microsphere and preparation method thereof

A technology of polyphosphazene and high temperature resistance, which is applied in the field of high temperature resistant polyphosphazene microspheres and its preparation, can solve the problems of single polyphosphazene microspheres and unsatisfactory thermal properties, and achieve simple and easy process and good thermal stability sexual effect

Inactive Publication Date: 2013-05-22
SHANGHAI JIAO TONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] At present, a large number of linear, grafted and cross-linked polyphosphazene materials have been synthesized, but cross-linked polyphosphazene microspheres are still relatively simple, and the patent of Zhu Lu et al. discloses a cross-linked polyphosphazene microsphere Synthesis, but it contains a large number of weak bonds, resulting in its thermal performance can not meet the application of some high-temperature occasions and other weaknesses

Method used

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  • High-temperature resistant polyphosphazene microsphere and preparation method thereof
  • High-temperature resistant polyphosphazene microsphere and preparation method thereof
  • High-temperature resistant polyphosphazene microsphere and preparation method thereof

Examples

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Comparison scheme
Effect test

Embodiment 1

[0024] Add 0.06 g (0.18 mmol) of hexachlorocyclotriphosphazene, 0.04 g (0.36 mmol) of phloroglucinol to a 100 mL flask, add 50 mL of acetonitrile to dissolve, and add 2 mL (1.44 mmol) when the temperature of the water bath reaches 30°C. Mol) triethylamine, reacted in an ultrasonic (190W) constant temperature water bath for 3h. After the reaction, the solid was separated by centrifugation. The crude product was washed three times with ethanol, then washed three times with deionized water, and finally dried in a vacuum oven for 24h. Get cross-linked polyphosphazene microspheres.

[0025] figure 1 Is the transmission electron micrograph of the crosslinked polyphosphazene microspheres, figure 2 Is a scanning electron micrograph of cross-linked polyphosphazene microspheres, image 3 It is a field emission scanning electron microscope photo of cross-linked polyphosphazene microspheres. It can be seen from the photo that the diameter of the microspheres is about 800 nm, and the surface ...

Embodiment 2

[0029] Using the equipment and preparation process described in Example 1, hexachlorocyclotriphosphazene was 0.06 g (0.18 mmol) and phloroglucinol was 0.06 g (0.54 mmol). The crude product was washed three times with ethanol, and then used Washed with deionized water three times, and finally dried in a vacuum oven for 24 hours to obtain cross-linked polyphosphazene microspheres. The analysis of the experimental results showed that the diameter of the microspheres was about 800nm, and the surface of the microspheres was flat and solid, and the structure was a cross-linked condensation structure of hexachlorocyclotriphosphazene and phloroglucinol.

Embodiment 3

[0031] Using the equipment and preparation process described in Example 1, the ultrasonic power used was 190W, the temperature of the constant temperature water bath was 30℃, and the reaction time was 1min, 10min, 30min, 1h, 2h, 3h, and some samples were taken out, and the samples were subjected to ethanol and deionization. Sample preparation after washing with water several times. The analysis of SEM experiment results showed that the diameter of the microspheres was 800nm-900nm, the surface of the microspheres was flat and solid, and the structure was a cross-linked condensation structure of hexachlorocyclotriphosphazene and phloroglucinol.

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Abstract

The invention relates to a high-temperature resistant polyphosphazene microsphere and a preparation method thereof and belongs to the organic micro-nanometer filed. The method comprises the following steps: performing reaction among hexachlorocyclopentadiene, phloroglucinol and triethylamine in an ultrasonic water bath environment to obtain a product; and washing the product, thereby obtaining the high-temperature resistant polyphosphazene microsphere. The high-temperature resistant polyphosphazene microsphere has a chemical structural formula shown in the specification. According to the microsphere and the method provided by the invention, the defects of the existing polymer microsphere preparation method and the existing polymer performance are overcome. Therefore, the polymer microsphere with better performance is synthetized by utilizing a simpler method.

Description

Technical field [0001] The invention relates to a material in the field of organic micro-nano and a preparation method thereof, in particular to a high-temperature resistant polyphosphazene microsphere and a preparation method thereof. Background technique [0002] In recent years, with the continuous deepening of nanotechnology research and the continuous expansion of various fields, as well as the excellent properties of polyphosphazene materials, polyphosphazene materials with micro-nano structures have increasingly attracted the attention of researchers. The micro / nano polyphosphazene material combines the high specific surface area of ​​the micro / nano material, which is easy to be organically modified, and obtains some excellent micro / nano materials. [0003] Polymer microsphere materials are widely used, such as plastic additives, coatings, adhesives, and building materials. In recent years, micro-nano polymer microsphere materials have gradually shown their applications in ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/6593
Inventor 潘亭军黄小彬唐小真
Owner SHANGHAI JIAO TONG UNIV
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