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Method for preparing degradable organic-inorganic nanometer hybrid material containing POSS (Polyhedral Oligomeric Silsesquioxanes)

A technology of inorganic nano and hybrid materials, which is applied in the field of preparation of degradable organic-inorganic nano hybrid materials, can solve the problems of poor dispersion of POSS particles and affect the performance of composite materials, so as to improve agglomeration, improve degradation performance, and promote scattered effect

Inactive Publication Date: 2011-11-16
NINGBO INST OF TECH ZHEJIANG UNIV ZHEJIANG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The results show that the introduction of POSS improves the thermal stability of the polymer to a certain extent, but because the size of POSS can be as small as nanometers, and the smaller the particle size, the easier it is to agglomerate itself. If only POSS is blended by physical The mode of adding, easily causes this agglomeration effect, makes POSS particles disperse poorly in matrix, thereby has influenced the further improvement of this composite performance (Wang RY, Wang SF, Zhang Y.Journal of Applied Polymer Science, 2009, 113:3095-3102)

Method used

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  • Method for preparing degradable organic-inorganic nanometer hybrid material containing POSS (Polyhedral Oligomeric Silsesquioxanes)
  • Method for preparing degradable organic-inorganic nanometer hybrid material containing POSS (Polyhedral Oligomeric Silsesquioxanes)
  • Method for preparing degradable organic-inorganic nanometer hybrid material containing POSS (Polyhedral Oligomeric Silsesquioxanes)

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] (1) Preparation of bifunctional POSS derivatives (II)

[0032]Add 8.74g of amino POSS (I) and 1.16g of hydroxyethyl acrylate into a three-necked flask filled with 100ml of dichloromethane, and stir vigorously for 72h at 20°C under normal pressure. After the reaction, the solution was distilled and purified to obtain the target product, the bifunctional POSS derivative (II), with a yield of 95%.

[0033] (2) Preparation of degradable organic-inorganic nano-hybrid copolyester containing POSS

[0034] 83.1g terephthalic acid, 90.1g 1,4-butanediol and 0.5wt% tetrabutyl titanate (Ti[OBu] 4 ) into a 250ml flask, at 200°C, under normal pressure (i.e. standard atmospheric pressure), magnetically stirred and reacted for 1 hour, then raised the temperature to 210°C, stirred at normal pressure for 0.5 hours, and stirred at 220°C for 0.5 hours at normal pressure, keeping the temperature constant Reduce the pressure to 20000Pa and continue the reaction for 3h to obtain a homogeneo...

Embodiment 2

[0036] (1) Preparation of bifunctional POSS derivatives (II)

[0037] Add 13.11 g of amino POSS (I) and 1.16 g of hydroxyethyl acrylate into a three-neck flask containing 150 ml of tetrahydrofuran, and stir vigorously for 48 h at 10° C. under normal pressure. After the reaction, the solution was distilled and purified to obtain the target product with a yield of 97%.

[0038] (2) Preparation of degradable organic-inorganic nano-hybrid copolyester containing POSS

[0039] 33.2g of phthalic acid, 76.1g of 1,3-propanediol (1:5) and 1.0wt% Ti[OBu] accounting for the total amount of the above two 4 Add it into a 250ml flask, stir it under normal pressure at 200°C for 1 hour, then raise the temperature to 215°C, stir it under normal pressure for 0.5 hour, then stir it under normal pressure at 230°C for 0.5 hour, keep the temperature constant and lower the pressure to 10000Pa, continue After reacting for 1.5h, a homogeneous, transparent and clear esterification product was obtained...

Embodiment 3

[0041] (1) Preparation of bifunctional POSS derivatives (II)

[0042] Add 10.48g of amino POSS (I) and 1.16g of hydroxyethyl acrylate into a three-necked flask filled with 200ml of acetone, and stir vigorously for 96h at 25°C under normal pressure. After the reaction, the solution was distilled and purified to obtain the target product with a yield of 97%.

[0043] (2) Preparation of degradable organic-inorganic nano-hybrid copolyester containing POSS

[0044] 75.5g terephthalic acid, 144.12g 1,4-cyclohexanedimethanol and 3.0wt% Ti[OBu] accounting for the total amount of the above two 4 Add it into a 250ml flask, stir it under normal pressure at 200°C for 1 hour, then raise the temperature to 210°C, stir it under normal pressure for 0.5 hour, then stir it under normal pressure at 220°C for 0.5 hour, keep the temperature constant and lower the pressure to 10000Pa, continue After 4 hours of reaction, a homogeneous, transparent and clear esterification product was obtained. Th...

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Abstract

The invention discloses a method for preparing a degradable organic-inorganic nanometer hybrid material containing POSS (Polyhedral Oligomeric Silsesquioxanes), comprising the following steps of: (1) firstly, preparing a difunctional POSS derivative (II) by carrying out the addition reaction of amino POSS (I) and 2-hydroxyethyl acrylate through Michael; and (2) secondly, forming an etherified product by carrying out the esterification reaction of aromatic dibasic acid and aliphatic dihydric alcohol and preparing the degradable organic-inorganic nanometer hybrid material containing the difunctional POSS through the melt polycondensation reaction of the difunctional POSS derivative (II) and aliphatic chydroxy oligomer with the etherified product. The preparation method has the advantages ofuniform dispersion and difficult agglomeration of POSS in the hybrid material during preparation, effective improvement on the performances of degradable copolyester composite material, simple operation and high yield.

Description

technical field [0001] The invention belongs to the technical field of degradable organic-inorganic nano hybrid composite materials, in particular to a preparation method of degradable organic-inorganic nano hybrid materials containing POSS. technical background [0002] With the continuous expansion of the application field and scale of polymer materials, the "white pollution" caused by waste polymer materials has become a worldwide public hazard that endangers the social environment and seriously hinders the sustainable development of the economy. Therefore, in recent years, degradable materials have become a research hotspot worldwide. Witt et al. reported in Macromolecular Chemistry and Physics, 1994,195:793-802 that aliphatic-aromatic copolyesters were synthesized using terephthalic acid, sebacic acid and propylene glycol as raw materials, and the experimental results showed that the copolyesters The degradation performance of polyester mainly depends on the molecular ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G63/695C08G63/78
Inventor 张艳王炳涛方征平郭正虹程捷
Owner NINGBO INST OF TECH ZHEJIANG UNIV ZHEJIANG
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