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Preparation method of high-nitrogen-content nitrified bamboo cellulose

A high nitrogen content, nitrobamboo technology, applied in the field of nitrocellulose preparation, can solve the problem that the nitrogen content of nitrocellulose does not reach high nitrogen content and the like, and achieve the effects of high nitrogen content, high purity and safety assurance

Active Publication Date: 2020-04-28
BEIJING INSTITUTE OF TECHNOLOGYGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

It can be seen that in these published patents, the nitrogen content of nitrocellulose has not reached the index of high nitrogen content

Method used

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  • Preparation method of high-nitrogen-content nitrified bamboo cellulose
  • Preparation method of high-nitrogen-content nitrified bamboo cellulose
  • Preparation method of high-nitrogen-content nitrified bamboo cellulose

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Half-immerse a pressure-resistant three-port device with a volume of 100mL and 50g of nitric acid with a concentration of 90% in a high-precision low-temperature constant temperature bath at -5°C, add 20g of acetic anhydride to the nitric acid, and start stirring at a rate of 500rpm. When the acetic anhydride is completely dissolved , add 5g of nitration aid to the solution, increase the temperature to 5°C, and keep it warm for 2 hours to obtain solution A; add 15g of bamboo cellulose to solution A, start stirring at a speed of 150rpm, and control the temperature at 15°C during stirring. ℃, after stirring for 40 minutes, seal the reaction device, replace the air in the reaction with nitrogen, after three replacements, raise the temperature to 25 ℃, keep warm for 6 hours, filter, and wash the filter residue with water 5 times to obtain 26.6g of nitrobamboo cellulose Crude;

[0026] The pressure-resistant three-port device with a volume of 2L and 399g of deionized water i...

Embodiment 2

[0031] Half-immerse a pressure-resistant three-port device with a volume of 300mL and 150g of nitric acid with a concentration of 95% in a high-precision low-temperature constant temperature tank at -5°C, add 50g of acetic anhydride to the nitric acid, and start stirring at a speed of 400rpm. When the acetic anhydride is completely dissolved , add 3g of nitration aid to the solution, increase the temperature to 6°C, and keep it warm for 2 hours to obtain solution A; add 30g of bamboo cellulose to solution A, start stirring at a speed of 170rpm, and control the temperature at 20°C during the stirring process ℃, after stirring for 35 minutes, seal the reaction device, replace the air in the reaction with nitrogen, after three replacements, raise the temperature to 28 ℃, keep warm for 4 hours, filter, and wash the filter residue with water 5 times to obtain 51.6g of nitrobamboo cellulose Crude;

[0032] The pressure-resistant three-port device with a volume of 5L and 877g of deio...

Embodiment 3

[0037]Half-immerse a pressure-resistant three-port device with a volume of 1000mL and 500g of nitric acid with a concentration of 98% in a high-precision low-temperature constant temperature tank at -5°C, add 200g of acetic anhydride to the nitric acid, and start stirring at a speed of 400rpm. When the acetic anhydride is completely dissolved , add 55g of nitration additive to the solution, increase the temperature to 10°C, and keep it warm for 1.5 hours to obtain solution A; add 135g of bamboo cellulose to solution A, start stirring at a rate of 200rpm, and control the temperature at 25°C during stirring. ℃, after stirring for 30 minutes, seal the reaction device, replace the air in the reaction with nitrogen, and after three replacements, raise the temperature to 30°C, keep it warm for 4 hours, filter, and wash the filter residue with water for 5 times to obtain 247g of crude nitrocellulose ;

[0038] The pressure-resistant three-port device with a volume of 15L and 3705g of...

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Abstract

The invention relates to a preparation method of high-nitrogen-content nitrified bamboo cellulose, and belongs to the field of nitrocellulose preparation. The method comprises the following steps: half-immersing a pressure-resistant three-opening device filled with nitric acid in a high-precision low-temperature constant-temperature tank, adding acetic anhydride into the nitric acid, stirring, adding a nitrification aid after complete dissolution, heating, and keeping the temperature to obtain a solution A; adding bamboo cellulose into the solution A, stirring for 20-40 minutes, sealing the reaction device, heating to 40-60 DEG C, keeping the temperature for 4-6 hours, filtering, and washing and drying filter residues to obtain a nitrified bamboo cellulose crude product; dissolving the crude product in water, and adding dilute sulfuric acid and a solution B; and filtering and drying to obtain the high-nitrogen-content nitrified bamboo cellulose. The preparation method disclosed by theinvention is simple in process, easily available in raw materials, low in waste acid discharge amount in the production process and suitable for factory operation; and the prepared product has high nitrogen content and meets the process parameter requirements of high-quality smokeless and sulfur-free pyrotechnic composition, propellant and explosive.

Description

technical field [0001] The invention relates to a method for preparing nitrocellulose with high nitrogen content, belonging to the field of nitrocellulose preparation. Background technique [0002] Nitrocellulose is obtained by esterifying cellulose with nitric acid. This process is simply called nitrification, more precisely oxynitrification. The nitration of cellulose can be expressed by the following equation: [0003] [0004] The chemical formula of cellulose in this equation simplifies to n=1 degree of polymerization. [0005] In a cellulose molecule, every six carbon atoms can be introduced (ONO 2 ) The maximum number of groups is three, and the theoretical nitrogen content in such nitrocellulose (trinitrate) is 14.15%. The nitrogen content of the experimental formula is C 6 h 10 o 5 The cellulose is calculated. In fact, if the terminal ring with a total of four hydroxyl groups is considered, the calculated theoretical maximum content will be slightly highe...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08B5/02C08B5/04
CPCC08B5/02C08B5/04
Inventor 刘吉平方祝青李年华吉伟生于保藏李琪军刘克普周耀明
Owner BEIJING INSTITUTE OF TECHNOLOGYGY
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