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Safe and efficient preparation method of polymer with high azide content

A polymer and nitrogen content technology, applied in the field of functional polymers, to achieve safe synthesis, fast and efficient synthesis, and avoid side reactions

Pending Publication Date: 2021-05-28
SHANGQIU NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the above work, the azide groups are all polymer end groups, and the azide group content in the polymer is very small; and the high azide content has higher requirements on the reaction conditions and azidation reagents. How to ensure the polymer functional Achieving a high conversion rate without changing the degree and molecular weight is a key issue in the synthesis of polymers with high azide content, and there is no relevant work report yet.

Method used

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  • Safe and efficient preparation method of polymer with high azide content
  • Safe and efficient preparation method of polymer with high azide content
  • Safe and efficient preparation method of polymer with high azide content

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Experimental program
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Embodiment 1

[0028] The preparation method of the high azide content polymer of the present embodiment is as follows:

[0029] Weigh 9.25g of polyepichlorohydrin (PECH, number average molecular weight 78400, molecular weight distribution index PDI=1.2), 12.7g of azidotrimethylsilane, and 100mL of anhydrous diglyme, and put them into a dry Schlenk bottle , liquid nitrogen freeze-thaw repeated three times and then filled with nitrogen protection. React under stirring at 60°C for 12 hours, pour into methanol for precipitation, filter and dry to obtain 9g polyazide glycidyl ether (GAP). The number average molecular weight is 82100, the molecular weight distribution index ID=1.26, and the conversion rate of azide group is 92%.

Embodiment 2

[0031] The preparation method of the high azide content polymer of the present embodiment is as follows:

[0032] Weigh 1.52g of poly-4-vinylbenzyl chloride (number-average molecular weight 12200, molecular weight distribution index PDI=1.16), 4.13g of diphenylphosphoryl azide, and 20mL of anhydrous toluene, put them into a dry Schlenk bottle, freeze and thaw with liquid nitrogen Vacuum was repeated three times and then filled with nitrogen for protection. React under stirring at 100° C. for 8 hours, pour into methanol / water mixture to precipitate, filter and dry to obtain 1.46 g of poly-4-azidomethylstyrene. The number average molecular weight is 12400, the molecular weight distribution index ID=1.2, and the azide group conversion rate is 96%.

Embodiment 3

[0034] The preparation method of the high azide content polymer of the present embodiment is as follows:

[0035] Weigh 0.25g of poly-3-bromohexylthiophene (number-average molecular weight 4400, molecular weight distribution index PDI=1.19), 0.67g of tributyltin azide, and 40mL of anhydrous xylene, add to a dry Schlenk bottle, freeze-thaw with liquid nitrogen and vacuumize After repeating three times, fill with nitrogen protection. React under stirring at 120°C for 6 hours, pour into methanol for precipitation, filter and dry to obtain 0.15 g of poly-3-azidohexylthiophene. The number average molecular weight is 3700, the molecular weight distribution index ID=1.16, and the azide group conversion rate is 99%.

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Abstract

The invention relates to a safe and efficient preparation method of a polymer with high azide content. According to the method, a polymer containing a carbon-halogen bond side chain is subjected to an azidation reaction in a non-polar solvent by adopting an azidation reagent of non-sodium azide. The adopted azide reagent has the characteristics of low sensitivity, low toxicity, good solubility and the like, the polymer with high azide content can be synthesized safely and efficiently at a high azide rate, and the molecular weight, molecular weight distribution and functionality are controllable. The prepared high-azide-content polymer can be used for click chemistry, photo-crosslinking materials, bio-orthogonal technologies, binders of high-energy solid propellants and the like.

Description

technical field [0001] The invention belongs to the technical field of functional polymers, and in particular relates to a safe and efficient preparation method for polymers with high azide content. Background technique [0002] Azide group is a functional group. In recent years, polymers with high azide content containing a large number of azide groups have been widely used in the fields of click chemistry, photocrosslinking materials, bioorthogonal technology, and high-energy solid propellants. Research. [0003] At present, the preparation of polymers with high azide content generally uses polymers containing easily leaving groups as precursors, and then reacts with sodium azide to obtain products. For example, Zhang et al. used poly-3,3-bisbromomethyloxetane as the precursor and sodium azide as the azidation reagent to efficiently synthesize poly-3,3-bis-azidomethyl Oxetanes (Journal of Energetic Materials, 2016, 34, 197-204). Zheng et al. used polyepichlorohydrin as ...

Claims

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Application Information

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IPC IPC(8): C08F8/32C08F112/14C08G61/12C08G65/333C08G65/336
CPCC08G65/336C08G65/33396C08G61/126C08F8/32C08G2650/04C08F112/18
Inventor 张弛张向飞翟滨孙家书臧运波
Owner SHANGQIU NORMAL UNIVERSITY