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Preparation method of amino polyphosphazene microspheres

A technology of amino polyphosphazene and microspheres is applied in the field of preparation of amino polyphosphazene microspheres, and can solve the problems of being unsuitable for large-scale production, difficult to remove dispersants or surfactants, complicated chemical synthesis steps, and the like, Achieve high thermal stability and good compatibility

Inactive Publication Date: 2010-01-13
SHANGHAI JIAO TONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In summary, the problems in the prior art are as follows: firstly, the target product contains dispersants or surfactants that are difficult to remove; secondly, the chemical synthesis steps are cumbersome and not suitable for large-scale production

Method used

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  • Preparation method of amino polyphosphazene microspheres
  • Preparation method of amino polyphosphazene microspheres
  • Preparation method of amino polyphosphazene microspheres

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] In a 250 ml flask, 0.32 g of hexachlorocyclotriphosphazene (HCCP) was dissolved in 160 ml of acetonitrile solvent, then 0.6 g of 4,4'-diaminodiphenyl ether (ODA) and 4 ml of acid-binding agent Triethylamine (TEA) was added to the above solution, and reacted for 8 hours under the condition of 40° C. and 150 watts of ultrasound. After the reaction, the crude product is filtered, washed with acetone and water for 2-3 times, and dried in a vacuum oven for 7-8 hours to prepare the target amino microspheres.

[0029] figure 1 , figure 2 It is the low magnification and high magnification scanning electron micrographs of the active microspheres prepared in Example 1. It can be seen from the photos that the surface of the microspheres is very clean, and there is no adhesion between the microspheres.

[0030] image 3 It is its transmission electron micrograph, and it can be known that the polymer microsphere has a solid structure.

[0031] Figure 4 It is the Fourier trans...

Embodiment 2

[0033] In a 250 ml flask, 0.32 g of hexachlorocyclotriphosphazene (HCCP) was dissolved in 110 ml of acetonitrile solvent, and then 0.6 g of 4,4'-diaminodiphenyl ether (ODA) and 4 ml of acid-binding The agent triethylamine (TEA) was added to the above solution, and reacted for 8 hours under the condition of 40 degrees and 150 watts of ultrasound. After the reaction, the crude product was filtered, washed with acetone and water for 2-3 times, and the product was dried in a vacuum oven for 7-8 hours to obtain functional amino microspheres with a clean surface (see Figure 5 ); the infrared spectrogram shows that its structure is 4,4-diaminodiphenyl ether and hexachlorocyclotriphosphazene cross-linked polycondensation structure.

Embodiment 3

[0035] In a 250 ml flask, 0.32 g of hexachlorocyclotriphosphazene (HCCP) was dissolved in 80 ml of acetonitrile solvent, and then 0.8 g of 4,4'-diaminodiphenyl ether (ODA) and 4 A milliliter of acid-binding agent triethylamine (TEA) was added to the above solution, and reacted for 8 hours under the condition of 40 degrees and 150 watts of ultrasound. After the reaction, the crude product was filtered, washed with acetone and water for 2-3 times, and after the product was dried in a vacuum oven for 7-8 hours, the functional amino microspheres with a clean surface (see Image 6 ); the infrared spectrogram shows that its structure is 4,4-diaminodiphenyl ether and hexachlorocyclotriphosphazene cross-linked polycondensation structure.

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Abstract

The invention relates to a preparation method of amino polyphosphazene microspheres, which belongs to the technical field of polymer materials. The preparation method comprises the steps of dispersing one part of hexachlorotriphosphazene and 0.5-2.5 parts of 4,4'-diaminodiphenyl ether in 195-390 parts of acetonitrile solution, adding 4.5-9 parts of acid binding agent in an organic solvent, then carrying out ultrasonic reaction for 8-10 hours at the temperature of 40-60 DEG C, preparing amino polyphosphazene suspension, filtering the amino polyphosphazene suspension after the ultrasonic reaction, carrying out repeated washing treatment, and finally drying for 7-8 hours through a vacuum baking oven, thereby preparing the amino polyphosphazene microspheres. The microspheres obtained by the preparation method have higher reductibility due to containing a large amount of aromatic ammonia, and can directly generate oxidation and reduction with chloroauric acid solution and load gold nanoparticles in situ. Meanwhile, the steps are simple, the preparation method does not need to add any stabilizer or surfactant, the post-treatment is further simple, and a byproduct of triethylamine salt is very easy to dissolve in water.

Description

technical field [0001] The invention relates to a preparation method in the technical field of polymer materials, in particular to a preparation method of amino polyphosphazene microspheres. Background technique [0002] Due to the designability of the structure and composition, the controllability of particle size and shape, large specific surface area, and strong surface adsorption, polymer microspheres have a wide range of applications in related fields such as adsorbents, latex diagnostics, drugs, and protein carriers. Applications. Polymer microspheres containing active amino groups are a very important class of functional materials, because amino groups have extremely high chemical reactivity and can be combined with a series of proteins and bioactive molecules. At present, dispersion polymerization and blending are mainly used to prepare the functional material. Dispersion polymerization is a special type of precipitation polymerization. At the beginning of the reac...

Claims

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Application Information

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IPC IPC(8): B01J13/14
Inventor 张鹏樊俊丽刘凤凤黄小彬唐小真
Owner SHANGHAI JIAO TONG UNIV
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