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Method for preparing shape-memory polyurethane by using hydroxylated peryleneimide

A technology of hydroxylated peryleneimide and polyurethane, which is applied in the field of intelligent polymer materials to achieve excellent thermal properties and simple operation

Active Publication Date: 2018-05-08
GUILIN UNIVERSITY OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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  • Method for preparing shape-memory polyurethane by using hydroxylated peryleneimide
  • Method for preparing shape-memory polyurethane by using hydroxylated peryleneimide
  • Method for preparing shape-memory polyurethane by using hydroxylated peryleneimide

Examples

Experimental program
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Effect test

Embodiment 1

[0019] (1) Take 3.92g 3,4,9,10-perylenetetracarboxylic dianhydride (PTCDA), 9.68g trishydroxymethylaminomethane (THAM), 1.83g anhydrous zinc acetate ((CH 3 COO) 2 Zn) and 100ml N-methylpyrrolidone (NMP) were added to a 250ml three-necked flask, heated to 80°C under nitrogen atmosphere, stirred and mixed for 15min, then continued to heat up to 155°C and stirred for 16h to obtain a dark purple solution.

[0020] (2) Suction filter the deep purple solution prepared in step (1), wash the filtrate 4 times with ethanol, and then put it in a vacuum oven at 50°C to dry for 10 hours, and the obtained purple powder is hydroxylated perylene imide, labeled as PBI.

[0021] (3) Put 2.0 g of polycaprolactone diol with a weight-average molecular weight of 1000 into a round-bottomed flask, heat to 80°C under a nitrogen atmosphere and magnetically stir until it melts, then add 10 ml of N,N-dimethyl Dibutyltin dilaurate (DBTDL) and 0.1 ml dibutyltin dilaurate (DBTDL), heat the mixture to 105 ...

Embodiment 2

[0026] (1) Take 3.92g 3,4,9,10-perylenetetracarboxylic dianhydride (PTCDA), 9.68g trishydroxymethylaminomethane (THAM), 1.83g anhydrous zinc acetate ((CH 3 COO) 2 Zn) and 100ml N-methylpyrrolidone (NMP) were added to a 250ml three-necked flask, heated to 80°C under nitrogen atmosphere, stirred and mixed for 15min, then continued to heat up to 155°C and stirred for 16h to obtain a dark purple solution.

[0027] (2) Suction filter the deep purple solution prepared in step (1), wash the filtrate 4 times with ethanol, and then put it in a vacuum oven at 50°C to dry for 10 hours, and the obtained purple powder is hydroxylated perylene imide.

[0028] (3) Put 2.0 g of polycaprolactone diol with a weight-average molecular weight of 1000 into a round-bottomed flask, heat to 80°C under a nitrogen atmosphere and magnetically stir until it melts, then add 10 ml of N,N-dimethyl Dibutyltin dilaurate (DBTDL) and 0.1 ml dibutyltin dilaurate (DBTDL), heat the mixture to 105 ° C for 15 min t...

Embodiment 3

[0033] (1) Take 3.92g 3,4,9,10-perylenetetracarboxylic dianhydride (PTCDA), 9.68g trishydroxymethylaminomethane (THAM), 1.83g anhydrous zinc acetate ((CH 3 COO) 2 Zn) and 100ml N-methylpyrrolidone (NMP) were added to a 250ml three-necked flask, heated to 80°C under nitrogen atmosphere, stirred and mixed for 15min, then continued to heat up to 155°C and stirred for 16h to obtain a dark purple solution.

[0034](2) Suction filter the deep purple solution prepared in step (1), wash the filtrate 4 times with ethanol, and then put it in a vacuum oven at 50°C to dry for 10 hours, and the obtained purple powder is hydroxylated perylene imide.

[0035] (3) Put 2.0 g of polycaprolactone diol with a weight-average molecular weight of 1000 into a round-bottomed flask, heat to 80°C under a nitrogen atmosphere and magnetically stir until it melts, then add 10 ml of N,N-dimethyl Dibutyltin dilaurate (DBTDL) and 0.1 ml dibutyltin dilaurate (DBTDL), heat the mixture to 105 ° C for 15 min to...

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Abstract

The invention discloses a method for preparing shape memory polyurethane by using hydroxylated perylene imide. Hydroxylated peryleneimides were first prepared using 3,4,9,10‑perylenetetracarboxylic dianhydride and trishydroxymethylaminomethane under a nitrogen atmosphere, and then hydroxylated peryleneimides were prepared using , polycaprolactone diol and hexamethylene diisocyanate were stirred and reacted at 80°C for 12 hours, then poured into a mold preheated at 50~80°C together, and heated and cured at 70~90°C for 10~14h , that is, the shape memory polyurethane is prepared. The method of the invention is simple to operate, and the prepared shape-memory polyurethane material has excellent thermal, mechanical and shape-memory properties. Its main performance indicators are as follows: elongation at break 600~1000%; tensile strength ≥ 20MPa; secondary cycle shape fixation rate 85% ~ 100%; secondary cycle shape recovery rate 90% ~ 100%; thermal decomposition The initial temperature is ≥250°C.

Description

technical field [0001] The invention belongs to the technical field of intelligent polymer materials, and in particular relates to a method for preparing shape-memory polyurethane by using hydroxylated perylene imide. Background technique [0002] Shape memory materials have important application value in the fields of biomedicine, structural parts and textiles, and have become a research hotspot and focus in academia and industry in recent years. In particular, shape memory polymer (Shape Memory Polymer, referred to as SMP) material has the advantages of easy processing, easy molding, light weight, etc., and has very huge potential application value. Since the 1980s, researchers from all over the world have increased their research on SMP. The investment and research of SMP have led to the rapid development of SMP research and become an important functional material at present. [0003] As one of the earliest materials to be used in the research and development of SMP, Sha...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G18/73C08G18/66C08G18/42C08G18/32C08G18/10
CPCC08G18/10C08G18/4277C08G18/73C08G2280/00C08G18/3846
Inventor 徐旭李裕琪陆绍荣韦春
Owner GUILIN UNIVERSITY OF TECHNOLOGY