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Azido polyether polyol and synthesis method thereof

A technology of polyol and nitrogen polyether, which is applied in the field of chemical synthesis of materials, can solve problems such as poor mechanical properties, and achieve the effects of overcoming poor mechanical properties, safe operation, and simple synthesis process

Inactive Publication Date: 2013-09-18
天元航材(营口)科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The reaction of the obtained azide polyether polyol product with di(or poly)isocyanate can directly form a network crosslinking structure, which can overcome the shortcomings of poor mechanical properties of hydroxyl-terminated azide polyether used in composite solid propellants

Method used

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  • Azido polyether polyol and synthesis method thereof
  • Azido polyether polyol and synthesis method thereof
  • Azido polyether polyol and synthesis method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Synthesis of 5-hydroxymethyl-1,2,3-triazole-azide polyether:

[0034] In a 500mL three-necked flask equipped with a thermometer, a reflux condenser and a constant pressure dropping funnel, add 200mL of dichloromethane and 35.8g of hydroxyl-terminated azide polyether-poly 3,3-bis(azidomethyl)oxa Cyclobutane / tetrahydrofuran copolymer, the reaction ratio adopts molar ratio, BAMO:THF=1:1. BAMO is the code name for 3,3-bis(azidomethyl)oxetane. After stirring to dissolve, the temperature was raised to 40°C. A solution formed by dissolving 1.1 g of propynyl alcohol-3 in 50 mL of dichloromethane was added dropwise. After 1 hour of addition, continue to keep warm for 6 hours. When the propynyl alcohol-3 in the reaction solution was detected by gas chromatography and completely disappeared, the reaction was stopped.

[0035] The reaction solution was directly evaporated to remove the solvent under reduced pressure, the distillation temperature was 40° C., and the vacuum degre...

Embodiment 2

[0041] Synthesis of 5-hydroxymethyl-1,2,3-triazole-azide polyether:

[0042] In a 500mL three-necked flask equipped with a thermometer, a reflux condenser and a constant pressure dropping funnel, add 80mL of chloroform and 35.8g of hydroxyl-terminated azide polyether-poly 3,3-bis(azidomethyl)oxetane The reaction ratio of alkane / tetrahydrofuran copolymer adopts molar ratio. BAMO:THF=1:1. After stirring to dissolve, the temperature was raised to 40°C. A solution of 4.6 g of propynyl alcohol-3 dissolved in 80 mL of dichloromethane was added dropwise. After 2 hours of addition, continue to keep warm for 8 hours. When the propynyl alcohol-3 in the reaction solution was detected by gas chromatography and completely disappeared, the reaction was stopped.

[0043] The reaction solution was directly evaporated to remove the solvent under reduced pressure, the distillation temperature was 40° C., and the vacuum degree was 45 mmHg. 39.9 g of yellow viscous product 5-hydroxymethyl-1,...

Embodiment 3

[0049] Synthesis of 5-hydroxymethyl-1,2,3-triazole-azide polyether:

[0050] In a 500mL three-neck flask equipped with a thermometer, a reflux condenser and a constant pressure dropping funnel, add 290mL of chloroform and 31.1g of poly-3,3-bis(azidomethyl)oxetane successively, stir and dissolve, and heat up to 50°C. A solution of 0.8 g of propynyl alcohol-3 dissolved in 50 mL of chloroform was added dropwise. After 1 hour of addition, continue to keep warm for 5 hours. When the propynyl alcohol-3 in the reaction solution was detected by gas chromatography and completely disappeared, the reaction was stopped.

[0051] The reaction solution was directly evaporated to remove the solvent under reduced pressure, the distillation temperature was 65° C., and the vacuum degree was 50 mmHg. 31.7 g of yellow viscous product 5-hydroxymethyl-1,2,3-triazole-azide polyether was obtained.

[0052] The product structural formula is as follows:

[0053]

[0054] Among them, p=16; q=3

...

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Abstract

The invention discloses an azido polyether polyol and a synthesis method thereof, belongs to the field of chemical synthesis of materials, and particularly relates to a method for synthesizing azido polyether polyol by using hydroxyl-terminated azido polyether and alkynol as raw materials and adopting 1,3-dipolar cycloaddition reaction. The azido polyether polyol is directly obtained by the 1,3-dipolar cycloaddition reaction of azido of azido polyether lateral group and alkynyl in alkynol. The azido polyether polyol is used for substituting azido polyether. In the molecular structure of the synthesized azido polyether polyol, the azido on the lateral group has high energy, so the azido is favorable for improving the energy of a composite solid propellant system; the azido polyether polyol also contains a plurality of reactive hydroxyls on the lateral group besides two terminal hydroxyls, so the azido polyether polyol used for synthesizing polyurethane can provide a cross-linked network structure, and the azido polyether polyol used for a composite solid propellant can provide good and adjustable mechanical property. The problem that the azido polyether polyol used for the composite solid propellant has poor mechanical property because the prepolymer generated by the reaction of the azido polyether and di (or poly) isocyanate has linear polymer structure is solved. Byproducts are not generated in the synthesis process of the azido polyether polyol; and the method has the advantages of simplicity in process, safety in operation and high reaction yield, and is suitable for industrial amplified production.

Description

technical field [0001] The invention belongs to the field of chemical synthesis of materials, specifically a method for synthesizing azide polyether polyols through 1,3-dipolar cycloaddition reaction using hydroxyl-terminated azide polyether and acetylenic alcohol as raw materials. Background technique [0002] Since the discovery of benzene azide and azido acid in the nineteenth century, azides have aroused great interest in the chemical community. For more than a hundred years, people have done extensive research on the synthesis methods, structure determination and applications of azides. Studies have shown that the energy of the azido group in the azide compound is very high, and each mole of the azide group can provide about 356kJ of heat of formation, so the compound containing the azide group has high energy. [0003] Because of this, azide polyether is widely used in composite solid propellants based on polyurethane. The polyurethane network structure formed by subs...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G65/331C08G18/48
Inventor 李战雄吕德斌
Owner 天元航材(营口)科技股份有限公司