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Shape memory polyurethane preparation method using hydroxylated perylene bisimide

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

Active Publication Date: 2017-03-15
GUILIN UNIVERSITY OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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  • Shape memory polyurethane preparation method using hydroxylated perylene bisimide
  • Shape memory polyurethane preparation method using hydroxylated perylene bisimide
  • Shape memory polyurethane preparation method using hydroxylated perylene bisimide

Examples

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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 shape memory polyurethane preparation method using hydroxylated perylene bisimide. The method comprises the steps of firstly under the nitrogen gas atmosphere, using 3, 4, 9, 10-tetracarboxylicaciddianhydride and trihydroxymethyl aminomethane to prepare hydroxylated perylene bisimide, then under the nitrogen gas atmosphere, stirring the prepared hydroxylated perylene bisimide with polycaprolactone diol and hexamethylene diisocyanate for reaction under 80 DEG C for 12 hours, pouring in a mold which is preheated to 50-80 DEG C, heating and curing for 10-14 hours under 70-90 DEG C to acquire the shape memory polyurethane. The method operation is simple. The prepared shape memory polyurethane has the advantages of being good in thermal, mechanical and memory properties. The major performance parameters are as following: the breaking elongation is 600-1000%; the tensile strength is larger than or equal to 20MPa; the secondary circulation shape fixing rate is 85-100%, the secondary circulation shape recovery rate is 90-100%, and the thermal decomposition starting temperature is larger than or equal to 250 DEG 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 Applications(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
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