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Preparation method of nitrified chitosan and application thereof

A technology of nitrating chitosan and chitosan, which is applied in the field of energetic materials and polymer materials, can solve the problems of nitrating chitosan performance and application research, low nitration substitution degree, etc., and achieve high substitution degree and nitration substitution degree The effect of improving and reducing the dosage

Active Publication Date: 2019-04-16
NORTHWEST UNIV(CN)
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] (1) In 1986, Shigehiro Hirano et al. reported nitrated chitosan, briefly discussed the preparation method and structural characterization of nitrated chitosan, but did not study the performance and application of nitrated chitosan
[0005] (2) Zhang Lina and others also prepared nitrated chitosan, but only used nitrated chitosan as an intermediate to synthesize a semi-interpenetrating network structure elastic material with polyester polyurethane, and the degree of nitrated substitution was low.

Method used

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  • Preparation method of nitrified chitosan and application thereof
  • Preparation method of nitrified chitosan and application thereof
  • Preparation method of nitrified chitosan and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0026] Add 3.0g of chitosan (deacetylation degree is 90%) to -3°C, 15mL of acetic anhydride, add 12mL of fuming nitric acid under stirring, then add 0.02mL of concentrated sulfuric acid, react at 2°C for 4h Stop the reaction, add 60 mL of ice water, filter and transfer the precipitate to saturated NaHCO 3 After soaking in the solution for 20 hours, filter, wash and dry in vacuum to obtain light yellow nitrated chitosan with a yield of 86%.

[0027] The elemental analysis result of the reactant obtained in this embodiment: C: 28.62%, H: 3.66%, N: 20.24%. The degree of nitration substitution is about 1.86. The impact sensitivity is >26J.

[0028] figure 1 It is the FT-IR curve chart of the chitosan of embodiment 1 and nitrated chitosan. The results show that: the three wavelengths (1642, 1270, 809cm) corresponding to the nitrate group (nitro) -1 ) exist, proving that nitrification has occurred.

Embodiment 2

[0030] Add 5.0g of chitosan (95% deacetylation degree) to -2°C, 20mL of acetic anhydride, add 25mL of fuming nitric acid under stirring, then add 0.04mL of concentrated sulfuric acid, and heat up to 2°C, react Stop the reaction after 5h, add 200mL of ice water, filter and transfer the precipitate into saturated NaHCO 3 After soaking in the solution for 24 hours, filtering, washing and vacuum drying, light yellow nitrated chitosan can be obtained with a yield of 84%.

[0031] The elemental analysis result of the reactant obtained in this embodiment: C: 29.55%, H: 3,35%, N: 16.50%. The nitrated substitution degree of nitrated chitosan was calculated to be about 2.01. The impact sensitivity is >21J.

[0032] figure 2 It is the DSC curve figure of the chitosan of embodiment 2 and nitrated chitosan. The results showed that chitosan had been nitrated and had a significant exothermic decomposition with a peak temperature of 192.55°C and an exothermic heat of 2200J / g.

[0033] ...

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Abstract

The invention relates to a preparation method of nitrified chitosan and application thereof. The related application is the application of nitrated chitosan as an energetic material, and the nitrification substitution degree of the nitrified chitosan is greater than 1.8. The related preparation method comprises the steps of adding chitosan into acetic anhydride according to the formula amount, adding fuming nitric acid in the stirring process, then adding concentrated sulfuric acid, executing reaction at a low temperature for a suitable time, and then conducting post-treatment on a reactant toobtain the nitrified chitosan. sugar. The nitrified chitosan prepared by the preparation method has large released decomposition heat amount and low sensitivity.

Description

technical field [0001] The invention belongs to the technical field of energetic materials and the field of polymer materials, in particular to a preparation method and application of nitrated chitosan. Background technique [0002] The existing nitrated chitosan is mainly used as an intermediate of elastic materials. [0003] The main method of the relevant preparation method of nitrated chitosan is as follows: adding appropriate amount of chitosan into concentrated nitric acid cooled by ice-salt water, adding acetic anhydride dropwise under mechanical stirring, and pouring the reaction solution into ice water to terminate the reaction after the reaction is completed. The obtained product has a nitration substitution degree of 0.8-1.5. For example: [0004] (1) In 1986, Shigehiro Hirano et al. reported nitrated chitosan, briefly discussed the preparation method and structural characterization of nitrated chitosan, but did not study the performance and application of nitra...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08B37/08C06B25/02
CPCC06B25/02C08B37/003
Inventor 徐抗震李楚平王为民冯治存杨燕京李辉赵凤起
Owner NORTHWEST UNIV(CN)
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