Amino acid spiral polysilane infrared absorption material and preparation method thereof

An amino acid-based, infrared absorption technology, applied in the field of amino acid-based helical polysilane infrared absorption materials and their preparation, can solve problems such as the destruction of side chain functional groups, harsh reaction conditions chlorosilane, etc., to improve unsaturation and thermal stability. , the effect of good solvent resistance

Active Publication Date: 2019-03-15
SOUTHEAST UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to its harsh reaction conditions and the reactive nature of chlorosilanes, the side chain functional groups are easily destroyed

Method used

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  • Amino acid spiral polysilane infrared absorption material and preparation method thereof
  • Amino acid spiral polysilane infrared absorption material and preparation method thereof
  • Amino acid spiral polysilane infrared absorption material and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] At 25°C under Ar atmosphere, add 60.00g of xylene and 3.48g of sodium metal into the reaction kettle, stir and disperse at 135°C for 1h, remove xylene by distillation under reduced pressure, drop to 25°C, add 60.00g of tetrahydrofuran, and add 6.09g of dichlorodecylhydrosilane, reacted at 25°C for 22h, added 360.00g of methanol to remove excess sodium metal, filtered, and washed the filter cake successively with 15.00g of water and methanol each time, washing 3 times to remove residual sodium methoxide, Vacuum drying at 25°C for 1 hour yielded 3.01 g of decylhydrogenpolysilane;

[0041] At 25°C, add 36.50g of L-glutamine and 50.00g of toluene into the reaction kettle, and add 48.50g of p-toluenesulfonic acid, then add 100.00g of allyl alcohol, heat up to reflux, react for 24h, and remove by distillation under reduced pressure. Propyl alcohol, toluene and water produced by reaction, add 100.00g of diethyl ether into the reaction kettle at 25°C, reflux for 0.5h, drop to 2...

Embodiment 2

[0044] At 25°C under Ar atmosphere, add 60.00g of xylene and 3.48g of sodium metal into the reaction kettle, stir and disperse at 135°C for 1h, remove xylene by distillation under reduced pressure, drop to 25°C, add 60.00g of tetrahydrofuran, and add 6.09g of dichlorodecylhydrosilane, reacted at 25°C for 22h, added 360.00g of methanol to remove excess sodium metal, filtered, and washed the filter cake successively with 15.00g of water and methanol each time, washing 3 times to remove residual sodium methoxide, Vacuum drying at 25°C for 1 hour yielded 3.01 g of decylhydrogenpolysilane;

[0045] At 25°C, add 36.50g of D-glutamine and 50.00g of toluene into the reaction kettle, add 48.50g of p-toluenesulfonic acid, then add 100.00g of allyl alcohol, heat up to reflux, react for 24h, and remove by distillation under reduced pressure. Propylene alcohol, toluene and water produced by reaction, add 100.00g diethyl ether into the reaction kettle at 25°C, reflux for 0.5h, drop to 25°C,...

Embodiment 3

[0048] At 25°C under Ar atmosphere, add 60.00g of xylene and 3.48g of sodium metal into the reaction kettle, stir and disperse at 135°C for 1h, remove xylene by distillation under reduced pressure, drop to 25°C, add 60.00g of tetrahydrofuran, and add 6.46g of dichloroundecylhydrosilane, reacted at 25°C for 22h, added 360.00g of methanol to remove excess sodium metal, filtered, washed the filter cake with 15.00g of water and methanol respectively, and washed 3 times to remove residual methanol Sodium, vacuum-dried at 25°C for 1 hour to obtain 3.26 g of undecylhydrogenpolysilane;

[0049] At 25°C, add 36.50g of L-lysine and 50.00g of toluene into the reaction kettle, and add 48.50g of p-toluenesulfonic acid, then add 100.00g of allyl alcohol, heat up to reflux, react for 24h, and remove by distillation under reduced pressure. Propyl alcohol, toluene and water produced by reaction, add 100.00g of diethyl ether into the reaction kettle at 25°C, reflux for 0.5h, drop to 25°C, filte...

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Abstract

The invention provides an amino acid spiral polysilane infrared absorption material and a preparation method thereof. The material is obtained through catalytic addition of L or D-2-amino acid propylene ester and alkyl hydrogen polysilane, the structural general formula of the material is as shown in the description. The degree of polymerization n is 10 to 5000; p is 10 to 12; and R1 is one of formulas as shown in the description. The glass transition temperature of the material is 35 to 70 DEG C, the thermal decomposition temperature is 300 to 450 DEG C, the absolute value of specific rotation is 10 to 70 degrees (25 DEG C), and the infrared emitting ability of 8 to 14 microns is 0.4 to 0.8 (25 DEG C). The material can be used for preparing infrared stealth materials, and can also be usedas a binder in continuous phases of photoelectric function materials.

Description

technical field [0001] The invention relates to an amino acid-based helical polysilane infrared absorbing material and a preparation method thereof, belonging to the preparation category of photoelectric functional polymer materials. Background technique [0002] Polysilane is a polymer whose main chain is composed of silicon atoms and has ring and linear configurations, wherein the linear configuration polysilane has a helical configuration. Since the main chain of polysilane is composed of σ-conjugated silicon atoms, a large conjugation effect similar to π electrons can be formed. The special electronic conjugation effect and polymer configuration make polysilane have unique photoelectric properties, which makes polysilane have broad application prospects in optoelectronic materials, nonlinear optical materials and low infrared emission materials. The Wurtz reaction is one of the most commonly used methods for preparing polysilanes. Carbon-functional polysilanes can be pr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/60
CPCC08G77/60
Inventor 周钰明张牧阳卜小海王泳娟何曼张一卫南秋利张雯君徐晓东
Owner SOUTHEAST UNIV
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