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High-nitrogen-content polymeric microsphere and preparation method thereof

A technology of microspheres and polyphosphazene, which is applied in the field of high nitrogen-containing polymer microsphere materials and its preparation, can solve the problems of low nitrogen content, low yield, long reaction preparation time, etc., and achieve the effect of increasing nitrogen content

Inactive Publication Date: 2015-04-08
SHANGHAI JIAO TONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the nitrogen content of this technology is low, the reaction preparation time is too long, and the yield is low

Method used

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  • High-nitrogen-content polymeric microsphere and preparation method thereof
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  • High-nitrogen-content polymeric microsphere and preparation method thereof

Examples

Experimental program
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Embodiment 1

[0016] This embodiment includes the following steps:

[0017] The first step is to react acetonitrile, triethylamine as an acid-binding agent, hexachlorocyclotriphosphazene, and triaminopyrimidine at 150°C for 3 hours, that is, 400 mg of hexachlorocyclotriphosphazene, triaminopyrimidine, and Pyrimidine is 288 mg, in a 200 mL digestion tank, add 60 mL of acetonitrile and 4 mL of triethylamine to the digestion tank in sequence.

[0018] The second step is to wait for the digestion tank to cool down to room temperature naturally in a drying oven; pour the product into a centrifuge tube, and use an ultrasonic cleaner to crush the product with large particles.

[0019] The third step is to centrifuge in a centrifuge at 7200 rpm for 5 minutes, then rinse with an organic solvent and centrifuge again, repeat three times; then dry at 80-100°C to obtain polymer microsphere materials.

[0020] Such as Figure 1 ~ Figure 3 Shown are the infrared spectrogram, thermogravimetric curve and ...

Embodiment 2

[0022] This embodiment includes the following steps:

[0023] The first step, react acetonitrile, triethylamine, hexachlorocyclotriphosphazene, and triaminopyrimidine at 150°C for 3 hours, that is, 200 mg of hexachlorocyclotriphosphazene and triaminopyrimidine are used for a single preparation. Pyrimidine is 144 mg. In a 200 mL digestion tank, add 60 mL of acetonitrile and 2 mL of triethylamine to the digestion tank in sequence.

[0024] The second step is to wait for the digestion tank to cool down to room temperature naturally in a drying oven; pour the product into a centrifuge tube, and use an ultrasonic cleaner to crush the product with large particles.

[0025] The third step is to centrifuge in a centrifuge at 7200 rpm for 5 minutes, then rinse with an organic solvent and centrifuge again, repeat three times; then dry at 80-100°C to obtain polymer microsphere materials.

Embodiment 3

[0027] This embodiment includes the following steps:

[0028] The first step, react acetonitrile, triethylamine, hexachlorocyclotriphosphazene and triaminopyrimidine at 150°C for 3 hours as an acid-binding agent, that is, the hexachlorocyclotriphosphazene used in a single preparation is 50-150 mg, Triaminopyrimidine is 36-108 mg, in a 200 mL digestion tank, add 60 mL of acetonitrile and 1-3 mL of triethylamine to the digestion tank in sequence.

[0029] The second step is to wait for the digestion tank to cool down to room temperature naturally in a drying oven; pour the product into a centrifuge tube, and use an ultrasonic cleaner to crush the product with large particles.

[0030] The third step is to centrifuge in a centrifuge at 7200 rpm for 5 minutes, then rinse with an organic solvent and centrifuge again, repeat three times; then dry at 80-100°C to obtain polymer microsphere materials.

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Abstract

The invention discloses a high-nitrogen-content polymeric microsphere and a preparation method thereof, relating to the technical field of polymer materials. A solvothermal method is adopted for replacing an ultrasonic method, and acetonitrile, triethylamine used as an acid-binding agent, phosphonitrilic chloride trimer and triaminopyrimidine are mixed and then subjected to a high-temperature and high-pressure reaction in a digestion tank; and after the reaction is completed, the product is cleaned and dried, so that a high-nitrogen-content polymeric microsphere material is obtained. According to the invention, a comonomer with a high nitrogen content is selected, so that the nitrogen content of products is increased; and in the prior art, the reaction can be completed in one day, but according to the invention, the reaction can be completed just in 1-3 hours, and a yield close to 100% can be achieved.

Description

technical field [0001] The invention relates to a technology in the field of polymer materials, in particular to a high nitrogen-containing polymer microsphere material and a preparation method thereof. Background technique [0002] Due to the unique morphology and performance of this microsphere material, it can be applied in carbon nitride structural material precursors, drug carriers, high-efficiency catalyst carriers, new optical materials, flame retardant materials, etc. [0003] After searching the prior art, it was found that Chinese Patent Document No. N101623613 was published (announced) on January 13, 2010, and disclosed a method for preparing aminopolyphosphazene microspheres in the technical field of polymer materials, including: adding 1 part of hexachloro Cyclic triphosphazene and 0.5-2.5 parts of 4,4'-diaminodiphenyl ether are dispersed in 195-390 parts of acetonitrile solution; 4.5-9 parts of acid-binding agent are added to the organic solvent, and then under...

Claims

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Application Information

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IPC IPC(8): C08G79/02C08G79/025
Inventor 黄小彬刘慈航刘飞雪朱宇诚陈奎永
Owner SHANGHAI JIAO TONG UNIV
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