CN111072785A - Preparation method of high-nitrogen-content nitrified bamboo cellulose - Google Patents
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- C08B5/00—Preparation of cellulose esters of inorganic acids, e.g. phosphates
- C08B5/02—Cellulose nitrate, i.e. nitrocellulose
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Abstract
The invention relates to a preparation method of high-nitrogen-content nitrated bamboo cellulose, belonging to the field of preparation of nitrated cellulose. Semi-immersing a pressure-resistant three-port device filled with nitric acid in a high-precision low-temperature constant-temperature tank, adding acetic anhydride into the nitric acid, stirring, adding a nitration auxiliary agent after complete dissolution, and heating and preserving heat to obtain a solution A. Adding the bamboo cellulose into the solution A, stirring for 20-40 minutes, sealing the reaction device, heating to 40-60 ℃, preserving heat for 4-6 hours, filtering, and washing and drying filter residues to obtain a crude product of the nitrated bamboo cellulose; dissolving the crude product in water and adding dilute sulfuric acid; and filtering and drying the solution B to obtain the nitrated bamboo cellulose with high nitrogen content. The preparation method has the advantages of simple process, easily obtained raw materials, less waste acid discharge in the production process and suitability for factory operation; the prepared product has high nitrogen content, and meets the technological parameter requirements of high-quality smokeless sulfur-free pyrotechnic compositions, propellant powder and explosive.
Description
Technical Field
The invention relates to a preparation method of high-nitrogen-content nitrated bamboo cellulose, belonging to the field of preparation of nitrated cellulose.
Background
Nitrocellulose is produced by esterifying cellulose with nitric acid. This process is simply referred to as nitrification, more specifically as continuous oxygen nitrification. The nitration of cellulose can be represented by the following equation:
the chemical formula of cellulose in this equation is simplified to a degree of polymerization n of 1.
Capable of being incorporated per six carbon atoms in one cellulose molecule (ONO)2) The maximum number of radicals is three, the theoretical nitrogen content in such nitrocellulose (trinitrate) being 14.15%. The nitrogen content is given by the empirical formula C6H10O5Calculated from the cellulose of (a). In fact, the calculated theoretical maximum content is somewhat higher, for example 14.17%, if terminal rings with a total of four hydroxyl groups are considered.
Nitrocellulose has the characteristics of easy dissolution in organic solvents, flammability and no smoke during combustion, and is widely applied to military and civil fields such as propellant, explosive, smokeless and sulfur-free pyrotechnic composition and the like. It is obtained by cellulose through nitration and esterification, and has the characteristic of simple production process.
At present, the raw material of nitrocellulose is mainly extracted from cotton and hemp, and bamboo fiber as the fifth natural cellulose has the characteristics of sufficient source, wide production area and high development speed, and can be used as a supplement and substitute of nitrocellulose raw material in the shortage of cotton and hemp.
Patent CN85106196A discloses a method for preparing nitrocellulose from Chinese alpine rush as raw material and mixed nitric acid and sulfuric acid as nitrating agent. The method can greatly shorten the nitration reaction time. The product yield is improved, and compared with the method using cotton linters as raw materials, the cost can be reduced by 21 percent. Patent CN1052484A discloses a method for preparing nitrocellulose from cotton stalks by hydrolyzing with white water to remove water-soluble substances and waxiness, saponifying with ternary mixed alkali solution to obtain cellulose, and using nitre, mixed sulfuric acid and nitrogen oxide as nitrating agents. The nitrogen content of the nitrocellulose prepared by the method is 12.2-13.5%. Patent CN103497076A discloses a method for preparing nitrocellulose powder by using waste paper, which is used for preparing gunpowder with low cost, high energy and small environmental pollution after combustion, and replacing black powder which is used in large quantity in the existing firework and cracker industry. The nitrogen content of the nitrocellulose prepared by the method is 10.72-13.16%. It can be seen that in none of these published patents, the nitrogen content of nitrocellulose has reached the index of high nitrogen content.
With the improvement of the quality of downstream products of the nitrocellulose, the market also puts higher requirements on the quality of the nitrocellulose. The production of nitrocellulose with excellent quality and high nitrogen content is one of the technical bottlenecks in the field of nitrocellulose preparation at home and abroad.
Disclosure of Invention
The invention aims to provide a preparation method of high-nitrogen-content nitrated bamboo cellulose, which realizes the safe preparation of the high-nitrogen-content bamboo cellulose. The bamboo cellulose with high nitrogen content has high purity, nitrogen elements are uniformly distributed, and the bamboo cellulose has high stability and combustion safety, so that the safety in the transportation and use processes is guaranteed.
The purpose of the invention is realized by the following technical scheme.
A preparation method of nitrified bamboo cellulose with high nitrogen content comprises the following steps:
step one, semi-immersing a pressure-resistant three-port device filled with nitric acid in a high-precision low-temperature constant-temperature tank at the temperature of-5-0 ℃, adding acetic anhydride into the nitric acid, wherein the mass ratio of the nitric acid to the acetic anhydride is (2-5): 1, stirring at the speed of 300-500 rpm, adding a nitration auxiliary agent into the solution after the acetic anhydride is completely dissolved, wherein the mass ratio of the nitration auxiliary agent to the nitric acid is (8-15), controlling the temperature to be increased to 5-10 ℃, and preserving the temperature for 1-2 hours to obtain a solution A. The concentration of the nitric acid is 90-98%.
Step two, adding bamboo cellulose into the solution A obtained in the step one, wherein the mass ratio of the bamboo cellulose to nitric acid is 1 (3-6), stirring is started at the speed of 150-200 rpm, the temperature is controlled at 15-25 ℃ in the stirring process, after stirring is carried out for 20-40 minutes, the reaction device is sealed, the air in the reaction is replaced by nitrogen, after the replacement is carried out for three times, the temperature is increased to 25-30 ℃, heat preservation is carried out for 4-6 hours, filtering is carried out, and filter residues are washed for 3-5 times by water to obtain a crude product of the nitrated bamboo cellulose;
step three, semi-immersing a pressure-resistant three-port device filled with a certain amount of deionized water in a high-precision constant-temperature tank, wherein a reflux condensing device is arranged on the pressure-resistant three-port device, adding the nitrated bamboo cellulose crude product obtained in the step two into the deionized water, wherein the mass ratio of the nitrated bamboo cellulose crude product to the deionized water is 1 (15-20), starting stirring at the speed of 50-100 rpm, heating the high-precision constant-temperature tank to 105-110 ℃, preserving heat for 10-20 minutes, adding a certain amount of dilute sulfuric acid with the concentration of 5-10%, wherein the mass ratio of the nitrated bamboo cellulose crude product to the dilute sulfuric acid is 1 (2-3), preserving heat for 10-20 minutes, adding a certain amount of solution B with the mass fraction of 2-4%, wherein the mass ratio of the nitrated bamboo cellulose crude product to the solution B is 1 (10-15), preserving heat for 30-60 minutes, and filtering, washing the filter residue with water for 3-5 times, and carrying out vacuum drying for 12-24 hours at the temperature of 20-40 ℃ to obtain the high-nitrogen-content nitrobamboo cellulose;
the nitration auxiliary agent in the first step comprises the following components in percentage by mass:
the preparation method of the nitration auxiliary agent comprises the following steps: will K2SO4、NH4NO3、KNO3And KH2PO4And (4) uniformly mixing.
In the third step, the solution B is one of sodium carbonate solution or sodium bicarbonate solution.
Advantageous effects
The preparation method of the nitrocellulose with high nitrogen content has the advantages of simple process, easily obtained raw materials, less waste acid discharge in the production process and suitability for factory operation; the prepared product has high purity, high nitrogen content and uniform nitrogen element distribution, meets the requirements of the technological parameters of high-quality smokeless sulfur-free pyrotechnic compositions, propellant powder and explosive, has higher stability and combustion safety, and ensures the safety in the transportation and use processes.
Detailed Description
The present invention will be further described with reference to the following examples.
Example 1
Semi-immersing a pressure-resistant three-port device with the volume of 100mL and containing 50g of 90% nitric acid in a high-precision low-temperature constant-temperature tank at the temperature of-5 ℃, adding 20g of acetic anhydride into the nitric acid, starting stirring at the speed of 500rpm, adding 5g of nitration auxiliary agent into the solution after the acetic anhydride is completely dissolved, raising the temperature to 5 ℃, and preserving the temperature for 2 hours to obtain a solution A; adding 15g of bamboo cellulose into the solution A, starting stirring at the speed of 150rpm, controlling the temperature at 15 ℃ in the stirring process, stirring for 40 minutes, sealing a reaction device, replacing air in the reaction with nitrogen, heating to 25 ℃ after three times of replacement, keeping the temperature for 6 hours, filtering, and washing filter residues with water for 5 times to obtain 26.6g of a crude product of the bamboo cellulose nitrate;
semi-immersing a pressure-resistant three-port device with the volume of 2L and containing 399g of deionized water in a high-precision constant-temperature tank, wherein a reflux condensing device is arranged on the pressure-resistant three-port device, adding 26.6g of crude nitrobamboo cellulose into the deionized water, starting stirring at the speed of 50rpm, heating the high-precision constant-temperature tank to 105 ℃, preserving heat for 10 minutes, adding 79.8g of dilute sulfuric acid with the concentration of 5%, preserving heat for 10 minutes, adding 266g of sodium carbonate solution with the mass fraction of 4%, preserving heat for 60 minutes, filtering, washing filter residues for 5 times with water, and performing vacuum drying at the temperature of 30 ℃ for 12 hours to obtain 27.8g of nitrobamboo cellulose with the nitrogen content of 14.01%;
the sample is subjected to an impact sensitivity test by using a 5kg drop weight, and the characteristic drop height of the sample is 65.72cm, which indicates that the sample has better impact stability; the sample nitrification mean square error is measured to be 1.9 by random sampling detection, which indicates that the sample has better nitrification uniformity.
The components and contents of the nitration auxiliary agent are as follows:
example 2
Semi-immersing a pressure-resistant three-port device with the volume of 300mL and containing 150g of 95% nitric acid in a high-precision low-temperature constant-temperature tank at the temperature of-5 ℃, adding 50g of acetic anhydride into the nitric acid, starting stirring at the speed of 400rpm, adding 3g of nitration auxiliary agent into the solution after the acetic anhydride is completely dissolved, raising the temperature to 6 ℃, and preserving the temperature for 2 hours to obtain a solution A; adding 30g of bamboo cellulose into the solution A, starting stirring at the speed of 170rpm, controlling the temperature at 20 ℃ in the stirring process, stirring for 35 minutes, sealing the reaction device, replacing the air in the reaction with nitrogen, heating to 28 ℃ after three times of replacement, keeping the temperature for 4 hours, filtering, and washing filter residues with water for 5 times to obtain 51.6g of a crude product of the bamboo cellulose nitrate;
semi-immersing a pressure-resistant three-port device with the volume of 5L and containing 877g of deionized water in a high-precision constant temperature tank, wherein a reflux condensing device is arranged on the pressure-resistant three-port device, adding 51.6g of a crude product of the nitrobamboo cellulose into the deionized water, starting stirring at the speed of 70rpm, heating the high-precision constant temperature tank to 107 ℃, preserving heat for 15 minutes, adding 129g of dilute sulfuric acid with the concentration of 8%, preserving heat for 15 minutes, adding 774g of a sodium carbonate solution with the mass fraction of 3%, preserving heat for 45 minutes, filtering, washing filter residues with water for 4 times, and performing vacuum drying at the temperature of 30 ℃ for 15 hours to obtain 55.8g of nitrobamboo cellulose with the nitrogen content of 14.04%;
the sample is subjected to an impact sensitivity test by using a 5kg drop weight, and the characteristic drop height of the sample is 66.57cm, which indicates that the sample has better impact stability; the sample nitrification mean square error is measured to be 1.7 through random sampling detection, which indicates that the sample has better nitrification uniformity.
The components and contents of the nitration auxiliary agent are as follows:
example 3
Semi-immersing a pressure-resistant three-port device with the volume of 1000mL and containing 500g of 98% nitric acid in a high-precision low-temperature constant-temperature tank with the temperature of-5 ℃, adding 200g of acetic anhydride into the nitric acid, starting stirring at the speed of 400rpm, adding 55g of nitration auxiliary agent into the solution after the acetic anhydride is completely dissolved, raising the temperature to 10 ℃, and preserving the temperature for 1.5 hours to obtain a solution A; adding 135g of bamboo cellulose into the solution A, starting stirring at the speed of 200rpm, controlling the temperature at 25 ℃ in the stirring process, stirring for 30 minutes, sealing the reaction device, replacing the air in the reaction with nitrogen, heating to 30 ℃ after three times of replacement, keeping the temperature for 4 hours, filtering, and washing filter residues with water for 5 times to obtain 247g of a crude product of the bamboo cellulose nitrate;
semi-immersing a pressure-resistant three-port device with the volume of 15L and containing 3705g of deionized water in a high-precision constant-temperature tank, wherein a reflux condensing device is arranged on the pressure-resistant three-port device, adding 247g of crude nitrobamboo cellulose into the deionized water, starting stirring at the speed of 100rpm, heating the high-precision constant-temperature tank to 110 ℃, preserving heat for 20 minutes, adding 494g of dilute sulfuric acid with the concentration of 6%, preserving heat for 20 minutes, adding 3211g of sodium bicarbonate solution with the mass fraction of 4%, preserving heat for 60 minutes, filtering, washing filter residues with water for 5 times, and performing vacuum drying at the temperature of 40 ℃ for 24 hours to obtain 251.6g of nitrobamboo cellulose with the nitrogen content of 14.07%; the sample is subjected to an impact sensitivity test by using a 5kg drop weight, and the characteristic drop height of the sample is 64.31cm, which indicates that the sample has better impact stability; the sample nitrification mean square error is measured to be 2.0 through random sampling detection, which indicates that the sample has better nitrification uniformity.
The components and contents of the nitration auxiliary agent are as follows:
the above detailed description is intended to illustrate the objects, aspects and advantages of the present invention, and it should be understood that the above detailed description is only exemplary of the present invention and is not intended to limit the scope of the present invention, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (2)
1. A preparation method of nitrified bamboo cellulose with high nitrogen content is characterized by comprising the following steps: the method comprises the following steps:
step one, semi-immersing a pressure-resistant three-port device filled with nitric acid in a high-precision low-temperature constant-temperature tank at the temperature of-5-0 ℃, adding acetic anhydride into the nitric acid, wherein the mass ratio of the nitric acid to the acetic anhydride is (2-5): 1, stirring at the speed of 300-500 rpm, adding a nitration auxiliary agent into the solution after the acetic anhydride is completely dissolved, wherein the mass ratio of the nitration auxiliary agent to the nitric acid is (8-15), controlling the temperature to be increased to 5-10 ℃, and preserving the temperature for 1-2 hours to obtain a solution A; the concentration of the nitric acid is 90-98%;
step two, adding bamboo cellulose into the solution A obtained in the step one, wherein the mass ratio of the bamboo cellulose to nitric acid is 1 (3-6), stirring is started at the speed of 150-200 rpm, the temperature is controlled at 15-25 ℃ in the stirring process, after stirring is carried out for 20-40 minutes, the reaction device is sealed, the air in the reaction is replaced by nitrogen, after the replacement is carried out for three times, the temperature is increased to 25-30 ℃, heat preservation is carried out for 4-6 hours, filtering is carried out, and filter residues are washed for 3-5 times by water to obtain a crude product of the nitrated bamboo cellulose;
step three, semi-immersing a pressure-resistant three-port device filled with a certain amount of deionized water in a high-precision constant-temperature tank, wherein a reflux condensing device is arranged on the pressure-resistant three-port device, adding the nitrated bamboo cellulose crude product obtained in the step two into the deionized water, wherein the mass ratio of the nitrated bamboo cellulose crude product to the deionized water is 1 (15-20), starting stirring at the speed of 50-100 rpm, heating the high-precision constant-temperature tank to 105-110 ℃, preserving heat for 10-20 minutes, adding a certain amount of dilute sulfuric acid with the concentration of 5-10%, wherein the mass ratio of the nitrated bamboo cellulose crude product to the dilute sulfuric acid is 1 (2-3), preserving heat for 10-20 minutes, adding a certain amount of solution B with the mass fraction of 2-4%, wherein the mass ratio of the nitrated bamboo cellulose crude product to the solution B is 1 (10-15), preserving heat for 30-60 minutes, and filtering, washing the filter residue with water for 3-5 times, and carrying out vacuum drying for 12-24 hours at the temperature of 20-40 ℃ to obtain the high-nitrogen-content nitrobamboo cellulose;
the nitration auxiliary agent in the first step comprises the following components in percentage by mass:
the preparation method of the nitration auxiliary agent comprises the following steps: will K2SO4、NH4NO3、KNO3And KH2PO4And (4) uniformly mixing.
2. The method for preparing the nitrified bamboo cellulose with high nitrogen content as claimed in claim 1, wherein the method comprises the following steps: in the third step, the solution B is one of sodium carbonate solution or sodium bicarbonate solution.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111647090A (en) * | 2020-07-14 | 2020-09-11 | 北京理工大学 | Method for nitrifying bamboo cellulose by using waste acid |
| CN112095344A (en) * | 2020-09-01 | 2020-12-18 | 北京理工大学 | Method for preparing fuse thread by directly nitrifying cotton thread |
| CN112159481A (en) * | 2020-09-01 | 2021-01-01 | 北京理工大学 | Preparation method of special nitrating agent for bamboo fiber |
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