3, 3-diazido methyl oxetane-ethylene glycol energetic copolyether with alternating multi-block structure and synthesis method thereof

A kind of technology of bis-azidomethyl oxetane and synthesis method, applied in 3 fields

Pending Publication Date: 2022-03-04
NANJING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, because ethylene oxide is easy to open the ring, it is difficult to achieve uniform copolymerization with butylene oxide monomers. At present, there is no research on BAMO-EG copolyether.

Method used

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  • 3, 3-diazido methyl oxetane-ethylene glycol energetic copolyether with alternating multi-block structure and synthesis method thereof
  • 3, 3-diazido methyl oxetane-ethylene glycol energetic copolyether with alternating multi-block structure and synthesis method thereof
  • 3, 3-diazido methyl oxetane-ethylene glycol energetic copolyether with alternating multi-block structure and synthesis method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] 1.05g of PBAMO (Mn=301, 3.5mmol) was dissolved in 10mL of THF, 2.24g of KOH (40mmol) was added, and the system was transferred to a constant temperature oil bath at 65°C. A THF solution of 1.12 g of tosylate-terminated polyethylene glycol (Mn=510, 2.2 mmol) was slowly dropped into the above reaction system, and the system continued to react at 65° C. for 24 h after the addition was completed. Then filter and rotary evaporate, the crude product was dissolved in dichloromethane, washed with distilled water until neutral. Then dried with anhydrous magnesium sulfate, suction filtered, and rotary evaporated, followed by adding petroleum ether with a boiling point of 60-90°C and methanol to wash and rotary evaporated to obtain a yellow sticky substance (0.78g)

[0024] Structure Identification:

[0025] FT-IR infrared: After PEG-OTS undergoes p-tosylation to obtain terminal tosylate polyethylene glycol, the infrared hydroxyl 3000-3500cm -1 disappear, proving that the end gr...

Embodiment 2

[0029] Dissolve 0.93g of PBAMO (Mn=301, 3.1mmol) in 20mL of THF, add 2.32g of KOH (41mmol), and transfer the system into a 65°C constant temperature oil bath. A THF solution of 1..01 g of tosylate-terminated glycerol (Mn=460, 2.2 mmol) was slowly dropped into the above reaction system, and the system continued to react at 65° C. for 24 h after the addition was completed. Then filter and rotary evaporate, the crude product was dissolved in dichloromethane, washed with distilled water until neutral. It was then dried over anhydrous magnesium sulfate, suction filtered, and rotary evaporated, followed by adding petroleum ether with a boiling point of 60-90°C and methanol for washing and rotary evaporation to obtain a yellow viscous substance (0.65 g).

Embodiment 3

[0031] Dissolve 0.95g of PBAMO (Mn=367, 2.6mmol) in 20mL of THF, add 2.01g of KOH (36mmol), and transfer the system into a 65°C constant temperature oil bath. A THF solution of 0.83 g of tosylate-terminated glycerol (Mn=460, 1.8 mmol) was slowly dropped into the above reaction system, and the system continued to react at 65° C. for 24 h after the addition was completed. Then filter and rotary evaporate, the crude product was dissolved in dichloromethane, washed with distilled water until neutral. It was then dried over anhydrous magnesium sulfate, suction filtered, and rotary evaporated, followed by adding petroleum ether with a boiling point of 60-90°C and methanol to wash and rotary evaporated to obtain a yellow sticky substance (0.52 g).

[0032] figure 1 The BAMO-EG alternating multi-block copolymer physical figure prepared for embodiment 1;

[0033] figure 2 For the Fourier transform infrared characteristic spectrogram of the BAMO-EG alternating multi-block copolymer ...

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Abstract

The invention discloses 3, 3-diazido methyl oxetane-ethylene glycol energetic copolyether with an alternating multi-block structure and a synthesis method thereof, the structural formula of an alternating multi-block energetic adhesive is shown as (I), m is equal to 1-4, n is equal to 1-4, l is equal to 1-4, k is equal to 1-10 and is an integer. The synthesis process comprises the following steps: by taking polyethylene glycol (PEG) and a 3, 3-diazido methyl oxetane homopolymer (PBAMO) as raw materials, carrying out Williamson ether synthesis to obtain the alternate multi-block azido energetic copolyether. The synthesis method is simple, and the alternating multi-block BAMO-EG energetic copolyether has an adjustable microscopic sequence structure and can endow a propellant with relatively good mechanical properties.

Description

technical field [0001] The invention relates to a 3,3-bis-azidomethyloxetane-ethylene glycol copolyether with an alternating multi-block structure and a synthesis method thereof. The compound can be used as an energetic binder of a solid propellant , belongs to the technical field of polymer materials. Background technique [0002] As an energetic adhesive with high nitrogen content, 3,3-bisazidomethyloxetane homopolymer (PBAMO) has the advantages of high energy, good compatibility and low mechanical sensitivity, and can greatly meet the energy requirements of energetic materials. However, the existence of PBAMO side groups hinders the chain rotation of the main chain and increases the crystallinity and glass transition temperature of the binder, thus making the solid propellant not resistant to low temperature and having poor toughness in a low temperature environment. [0003] In order to solve the problem of low-temperature embrittlement of PBAMO, researchers introduced...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/333C06D5/06C06B23/00
CPCC08G65/33396C06D5/06C06B45/105
Inventor 郑文芳李雅楠李文希潘仁明蔺向阳
Owner NANJING UNIV OF SCI & TECH
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