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3, 3-diazidomethyl oxetane-tetrahydrofuran energetic copolyether with alternating multi-block structure and synthesis method thereof

A technology of diazidomethyl oxetane and tetrahydrofuran is applied in 3 fields, and can solve the problems such as the inability to obtain alternating multi-block copolymerization and the need for further optimization of the microscopic sequence structure.

Active Publication Date: 2021-11-09
NANJING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, cationic random copolymerization cannot obtain more controllable alternating multi-block copolymerization, and the microscopic sequence structure needs to be further optimized

Method used

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  • 3, 3-diazidomethyl oxetane-tetrahydrofuran energetic copolyether with alternating multi-block structure and synthesis method thereof
  • 3, 3-diazidomethyl oxetane-tetrahydrofuran energetic copolyether with alternating multi-block structure and synthesis method thereof
  • 3, 3-diazidomethyl oxetane-tetrahydrofuran energetic copolyether with alternating multi-block structure and synthesis method thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] 1.2g of PBAMO (Mn=322, 3.7mmol) 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 1.2 g of tosylate-terminated polytetrahydrofuran (Mn=542, 2.2 mmol) was slowly dropped into the above reaction system. After the dropwise addition, the system continued to react at 65°C for 18 hours. Then filter and rotary evaporate, the crude product was dissolved in dichloromethane, washed with distilled water until neutral. Then dry with anhydrous magnesium sulfate, filter with suction, and rotary evaporate, then add petroleum ether with a boiling point of 60-90°C and methanol to wash and rotary evaporate to obtain a yellow viscous substance (0.82g)

[0026] Structure Identification:

[0027] FT-IR infrared: After polytetrahydrofuran is p-tosylated to obtain terminal tosylate polytetrahydrofuran, the infrared hydroxyl 3000-3500cm -1 disappear, proving that the end group of PTHF ha...

Embodiment 2

[0031] 1.5g of PBAMO (Mn=448, 3.3mmol) was dissolved in 20mL of THF, 2.57g of KOH (40mmol) was added, and the system was transferred to a constant temperature oil bath at 65°C. A THF solution of 1.2 g of tosylate-terminated polytetrahydrofuran (Mn=542, 2.2 mmol) was slowly dropped into the above reaction system, and the reaction was continued 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 (0.74 g).

Embodiment 3

[0033] 1.28g of PBAMO (Mn=510, 2.5mmol) was dissolved in 20mL of THF, 2.01g of KOH (40mmol) was added, and the system was transferred to a 65°C constant temperature oil bath. A THF solution of 0.8 g of tosylate-terminated 1,4-butanediol (Mn=398, 2.0 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 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 (0.52 g).

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Abstract

The invention discloses 3, 3-diazidomethyl oxetane-tetrahydrofuran energetic copolyether with an alternating multi-block structure and a synthesis method thereof, wherein the structural formula of the alternating multi-block energetic adhesive is shown as (I), m is equal to 1-5, n is equal to 1-4, k is equal to 1-10, and m, n and k are integers. The synthesis process comprises the following steps: by taking polytetrahydrofuran (PTHF) and a 3, 3-diazidomethyl oxetane homopolymer (PBAMO) as raw materials, carrying out Williamson ether synthesis to obtain the alternating multi-block azido energetic adhesive. The synthesis method is simple, and the alternating multi-block BAMO-THF energetic adhesive 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-tetrahydrofuran copolymer with an alternating multi-block structure and a synthesis method thereof. The compound can be used as an energetic binder of a solid propellant and belongs to Polymer material technology field. Background technique [0002] 3,3-Bisazidomethyloxetane homopolymer (PBAMO), as a high nitrogen content energetic binder, has high heat of formation, high energy, good compatibility and low mechanical sensitivity, etc. It is one of the research hotspots in the field of energetic adhesives and one of the future development directions. PBAMO increases energy by introducing azide groups into carbon chain side groups, but the presence of side groups will increase the glass transition temperature of the binder, making solid propellants not resistant to low temperatures and poor toughness in low temperature environments. [0003] In order to solve the problem of low-temperature embrittle...

Claims

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Application Information

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IPC IPC(8): C08G65/333C08G65/334C08G81/00C06B45/10
CPCC08G65/33396C08G65/3346C08G81/00C06B45/105C08G2170/00
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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