CN113307708B - Preparation method of single-base powder and single-base powder obtained by method - Google Patents
Preparation method of single-base powder and single-base powder obtained by method Download PDFInfo
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- CN113307708B CN113307708B CN202110669239.8A CN202110669239A CN113307708B CN 113307708 B CN113307708 B CN 113307708B CN 202110669239 A CN202110669239 A CN 202110669239A CN 113307708 B CN113307708 B CN 113307708B
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- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
- C06B21/00—Apparatus or methods for working-up explosives, e.g. forming, cutting, drying
- C06B21/0033—Shaping the mixture
- C06B21/0066—Shaping the mixture by granulation, e.g. flaking
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- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
- C06B25/00—Compositions containing a nitrated organic compound
- C06B25/18—Compositions containing a nitrated organic compound the compound being nitrocellulose present as 10% or more by weight of the total composition
- C06B25/20—Compositions containing a nitrated organic compound the compound being nitrocellulose present as 10% or more by weight of the total composition with a non-explosive or a non-explosive or a non-thermic component
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Abstract
The invention discloses a preparation method of single-base powder and the single-base powder obtained by the method, the preparation method of the single-base powder comprises the following mixing steps: dissolving the base material with an organic solvent, adding a stabilizer, and then adding nitrocellulose to obtain a mixture; the base material is at least one of nitrocotton, single-base tubular medicine, single-base powder, double-base tubular medicine and double-base powder; a forming step: pressing and vacuum-filtering the mixture to obtain a solid material; and (3) pelletizing: immersing the solid material into water, and granulating to obtain single-base powder; the preparation method effectively removes water and solvent in the single-base powder, and has the advantages of simple production process, good quality of the single-base powder, easy combustion and large energy.
Description
Technical Field
The invention relates to a preparation method of single-base powder and the single-base powder obtained by the method, belonging to the technical field of chemical product preparation.
Background
The single-base powder used in the market at present is a powder material with 40-100 meshes obtained by crushing a military-retired single-base pipe with water, but the raw material source is limited, and the market demand cannot be met. The existing industrial method for producing the single-base powder adopts the processes of emulsifying and plasticizing nitrocotton, for example, ethyl acetate and the like are used as solvents to be emulsified and solidified in water, the product is bound to wrap the water and the solvents and cannot be removed, the process is complex, the production efficiency is low, the prepared powder product still contains the water and the solvents after being dried, the combustion speed of the product is low, the product is not easy to store, and the quality requirement cannot be met. Thus, there is still much room for improvement in the production of single-base powders.
Disclosure of Invention
In order to overcome the defects of the prior art, the first object of the invention is to provide a preparation method of the single-base powder, which effectively removes water and solvent in the single-base powder, has simple production process, good quality of the single-base powder, easy combustion and large energy.
The second purpose of the invention is to provide a single-base powder obtained by the method, which is inflammable and smokeless and has good safety.
The first purpose of the invention can be achieved by adopting the following technical scheme: a method for preparing single-base powder comprises,
mixing: dissolving the base material with an organic solvent, adding a stabilizer, and then adding nitrocellulose to obtain a mixture; the base material is at least one of nitrocotton, single-base tubular medicine, single-base powder, double-base tubular medicine and double-base powder;
a forming step: pressing and vacuum-filtering the mixture to obtain a solid material;
and (3) pelletizing: and (3) immersing the solid material into water, and granulating to obtain the single-base powder.
Further, in the mixing step, the base material is at least one of nitrocotton, single-base tubular medicine, single-base powder, double-base tubular medicine, double-base powder and celluloid.
Further, in the mixing step, the organic solvent is at least one of alcohols, ketones and ethers.
Further, in the mixing step, the stabilizer is diphenylamine.
Further, in the mixing step, the ratio of the weight of the binder to the volume of the organic solvent is 1g (4-15) mL.
Further, in the mixing step, the weight ratio of the base material to the stabilizer is 10 (0.3-2).
Further, in the mixing step, after the base material is dissolved, the weight ratio of the added nitrocellulose to the base material is (2-5): 1.
Further, in the granulating step, the organic solvent in the water is recovered by calcium chloride or distillation after the granulation.
Further, in the granulating step, the grain diameter of the granules is 20-150 meshes.
The second purpose of the invention can be achieved by adopting the following technical scheme: a single-base powder is prepared by the method.
The design principle of the invention is as follows:
and the excess organic solvent is extracted by vacuum filtration in the molding step, so that the solvent in the produced product is less. The pelletizing step is also a solidification and desolventizing process: by granulating in water, wherein the nitrocotton is non-absorbent and insoluble in water, and the organic solvent can be solidified when meeting water, when the nitrocotton is granulated, water permeates from outside to inside, so that the surface of the organic solvent is solidified to form a porous shape, a water inlet and outlet channel is opened, water can be sucked out during drying, and the obtained single-base powder has higher density; and because the grain cutting is carried out in water, the safety in the production process is greatly improved.
Compared with the prior art, the invention has the beneficial effects that:
1. the preparation method has the advantages that the raw materials are easy to obtain, water and a solvent in the single-base powder can be effectively removed in the preparation process, the production process is simple and safe, and large-scale production can be realized;
2. in the granulating step, the single-base powder forms a porous structure, the dried finished product does not contain water or organic solvent, the nitrocotton cannot be torn in the granulating process, burrs cannot be generated, and the use requirement can be met;
3. the method can recover the organic solvent through suction filtration, and the organic solvent can be recycled, so that the method is environment-friendly in production;
4. the single-base powder obtained by the invention has good quality, easy combustion, no smoke and large energy.
Detailed Description
The invention will be further described with reference to specific embodiments:
a method for preparing single-base powder comprises,
mixing: dissolving the base material with an organic solvent, adding a stabilizer, and then adding nitrocellulose to obtain a mixture;
the base material is at least one of nitrocotton, single-base tubular medicine, single-base powder, double-base tubular medicine, double-base powder and celluloid;
the organic solvent is at least one of alcohols, ketones and ethers;
the stabilizer is diphenylamine; the stabilizer has the function of improving the safety of the single-base powder in the processes of production, transportation and storage;
the ratio of the weight of the base material to the volume of the organic solvent is 1g (4-15) mL;
the weight ratio of the base material to the stabilizer is 10 (0.3-2);
the weight ratio of the added nitrocellulose to the base material is (2-5) to 1;
a forming step: putting the mixture into equipment with a hole at the bottom and a vacuum at the lower part, pressurizing the top, and performing suction filtration below the equipment at the same time to obtain a solid material; the suction filtration is used for removing the redundant organic solvent and can be recycled;
and (3) pelletizing: and (3) immersing the solid material into water, granulating, wherein the grain size of the granules is 20-150 meshes, and recovering the organic solvent in the water by using a calcium chloride or distillation method after the granules are granulated.
The water removed in the granulating step can be recycled, and the production process is environment-friendly.
Example 1:
a method for preparing single-base powder comprises,
mixing: dissolving 100g of anhydrous nitrocotton by 900mL of anhydrous ethanol and 100mL of acetone, adding 5g of diphenylamine, and then adding 300g of nitrocellulose to obtain a mixture;
a molding step: putting the mixture into equipment with a hole at the bottom and a vacuum at the lower part, pressurizing the top, and performing suction filtration below the equipment at the same time to obtain a solid material;
and (3) pelletizing: and (3) immersing the solid material into water, granulating, wherein the grain size of the granules is 85 meshes, and recovering the organic solvent in the water by using calcium chloride after the granules are granulated.
Example 2:
a method for preparing single-base powder comprises,
mixing: dissolving 100g of anhydrous nitrocotton by 800mL of anhydrous ethanol and 100mL of acetone, adding 5g of diphenylamine, and then adding 400g of nitrocellulose to obtain a mixture;
a forming step: putting the mixture into equipment with a hole at the bottom and vacuum at the lower part, pressurizing the top, and performing suction filtration at the lower part at the same time to obtain a solid material;
and (3) pelletizing: and (3) immersing the solid material into water, granulating, wherein the grain diameter of the granules is 85 meshes, and recovering the organic solvent in the water by using calcium chloride after the granules are granulated.
Example 3:
a method for preparing single-base powder comprises,
mixing: dissolving 100g of double-base tubular medicine by 850mL of absolute ethyl alcohol and 100mL of acetone, adding 5g of diphenylamine, and then adding 400g of nitrocellulose to obtain a mixture;
a forming step: putting the mixture into equipment with a hole at the bottom and a vacuum at the lower part, pressurizing the top, and performing suction filtration below the equipment at the same time to obtain a solid material;
and (3) pelletizing: and (3) immersing the solid material into water, granulating, wherein the grain size of the granules is 85 meshes, and recovering the organic solvent in the water by using calcium chloride after the granules are granulated.
Example 4:
a method for preparing single-base powder comprises,
mixing: dissolving 50g of nitrocotton and 50g of celluloid in 900mL of anhydrous methanol and 200mL of acetone, adding 8g of diphenylamine, and then adding 350g of nitrocellulose to obtain a mixture;
a forming step: putting the mixture into equipment with a hole at the bottom and a vacuum at the lower part, pressurizing the top, and performing suction filtration below the equipment at the same time to obtain a solid material;
and (3) pelletizing: and (3) immersing the solid material into water, granulating, wherein the grain size of the granules is 85 meshes, and recovering the organic solvent in the water by using calcium chloride after the granules are granulated.
Example 5:
a method for preparing single-base powder comprises,
mixing: dissolving 100g of double-base tubular medicine and 40g of celluloid in 500mL of absolute ethyl alcohol, 150mL of absolute methanol and 200mL of acetone, adding 5g of diphenylamine, and then adding 400g of nitrocellulose to obtain a mixture;
a forming step: putting the mixture into equipment with a hole at the bottom and a vacuum at the lower part, pressurizing the top, and performing suction filtration below the equipment at the same time to obtain a solid material;
and (3) pelletizing: and (3) immersing the solid material into water, granulating, wherein the grain diameter of the granules is 95 meshes, and recovering the organic solvent in the water by using calcium chloride after the granules are granulated.
Example 6:
a method for preparing single-base powder comprises,
mixing: dissolving 100g of double-base tubular medicine and 40g of celluloid in 400mL of absolute ethyl alcohol, 100mL of absolute methanol and 150mL of acetone, adding 6g of diphenylamine, and then adding 500g of nitrocellulose to obtain a mixture;
a forming step: putting the mixture into equipment with a hole at the bottom and a vacuum at the lower part, pressurizing the top, and performing suction filtration below the equipment at the same time to obtain a solid material;
and (3) pelletizing: and (3) immersing the solid material into water, granulating, wherein the grain diameter of the granules is 95 meshes, and recovering the organic solvent in the water by using calcium chloride after the granules are granulated.
Example 7:
a method for preparing single-base powder comprises,
mixing: dissolving 100g of single-base tubular medicine by using 450mL of absolute ethyl alcohol and 120mL of acetone, adding 4g of diphenylamine, and then adding 400g of nitrocellulose to obtain a mixture;
a molding step: putting the mixture into equipment with a hole at the bottom and a vacuum at the lower part, pressurizing the top, and performing suction filtration below the equipment at the same time to obtain a solid material;
and (3) pelletizing: and (3) immersing the solid material into water, granulating, wherein the grain diameter of the granules is 95 meshes, and recovering the organic solvent in the water by using calcium chloride after the granules are granulated.
The fire transfer speed detection is carried out on the embodiments 1 to 7, the cake fireworks are prepared for the combustion time and speed detection, and the proportion of the cake fireworks is as follows: 12 wt% ammonium perchlorate, 4 wt% titanium sponge, 84 wt% single base powder, 5.5g total weight, results are shown in Table 1:
TABLE 1 test results of examples 1 to 7
Various other changes and modifications to the above-described embodiments and concepts will become apparent to those skilled in the art from the above description, and all such changes and modifications are intended to be included within the scope of the present invention as defined in the appended claims.
Claims (8)
1. A method for preparing single-base powder is characterized by comprising the following steps,
mixing: dissolving 100g of anhydrous nitrocotton by 900mL of anhydrous ethanol and 100mL of acetone, adding 5g of diphenylamine, and then adding 300g of nitrocellulose to obtain a mixture;
a forming step: putting the mixture into equipment with a hole at the bottom and a vacuum at the lower part, pressurizing the top, and performing suction filtration below the equipment at the same time to obtain a solid material;
and (3) pelletizing: immersing the solid material into water, granulating, wherein the particle size of the granules is 85 meshes, and recovering the organic solvent in the water by using calcium chloride after the granules are granulated;
the preparation method has no emulsification step.
2. A method for preparing single-base powder is characterized by comprising the following steps,
mixing: dissolving 100g of anhydrous nitrocotton by 800mL of anhydrous ethanol and 100mL of acetone, adding 5g of diphenylamine, and then adding 400g of nitrocellulose to obtain a mixture;
a molding step: putting the mixture into equipment with a hole at the bottom and a vacuum at the lower part, pressurizing the top, and performing suction filtration below the equipment at the same time to obtain a solid material;
and (3) pelletizing: immersing the solid material into water, granulating, wherein the particle size of the granules is 85 meshes, and recovering the organic solvent in the water by using calcium chloride after the granules are granulated;
the preparation method has no emulsification step.
3. A method for preparing single-base powder is characterized by comprising the following steps,
mixing: dissolving 100g of double-base tubular medicine by 850mL of absolute ethyl alcohol and 100mL of acetone, adding 5g of diphenylamine, and then adding 400g of nitrocellulose to obtain a mixture;
a forming step: putting the mixture into equipment with a hole at the bottom and a vacuum at the lower part, pressurizing the top, and performing suction filtration below the equipment at the same time to obtain a solid material;
and (3) pelletizing: immersing the solid material into water, granulating, wherein the particle size of the granules is 85 meshes, and recovering the organic solvent in the water by using calcium chloride after the granules are granulated;
the preparation method has no emulsification step.
4. A method for preparing single-base powder is characterized by comprising the following steps,
mixing: dissolving 50g of nitrocotton and 50g of celluloid in 900mL of anhydrous methanol and 200mL of acetone, adding 8g of diphenylamine, and then adding 350g of nitrocellulose to obtain a mixture;
a forming step: putting the mixture into equipment with a hole at the bottom and a vacuum at the lower part, pressurizing the top, and performing suction filtration below the equipment at the same time to obtain a solid material;
and (3) pelletizing: immersing the solid material into water, granulating, wherein the particle size of the granules is 85 meshes, and recovering the organic solvent in the water by using calcium chloride after the granules are granulated;
the preparation method has no emulsification step.
5. A method for preparing single-base powder is characterized by comprising the following steps,
mixing: dissolving 100g of double-base tubular medicine and 40g of celluloid in 500mL of absolute ethyl alcohol, 150mL of absolute methanol and 200mL of acetone, adding 5g of diphenylamine, and then adding 400g of nitrocellulose to obtain a mixture;
a forming step: putting the mixture into equipment with a hole at the bottom and a vacuum at the lower part, pressurizing the top, and performing suction filtration below the equipment at the same time to obtain a solid material;
and (3) pelletizing: immersing the solid material into water, cutting into particles, wherein the particle size of the cut particles is 95 meshes, and recovering the organic solvent in the water by using calcium chloride after cutting into particles;
the preparation method has no emulsification step.
6. A method for preparing single-base powder is characterized by comprising the following steps,
mixing: dissolving 100g of double-base tubular medicine and 40g of celluloid in 400mL of absolute ethyl alcohol, 100mL of absolute methanol and 150mL of acetone, adding 6g of diphenylamine, and then adding 500g of nitrocellulose to obtain a mixture;
a forming step: putting the mixture into equipment with a hole at the bottom and a vacuum at the lower part, pressurizing the top, and performing suction filtration below the equipment at the same time to obtain a solid material;
and (3) pelletizing: immersing the solid material into water, cutting into particles, wherein the particle size of the cut particles is 95 meshes, and recovering the organic solvent in the water by using calcium chloride after cutting into particles;
the preparation method has no emulsification step.
7. A method for preparing single-base powder is characterized by comprising the following steps,
mixing: dissolving 100g of single-base tubular medicine by using 450mL of absolute ethyl alcohol and 120mL of acetone, adding 4g of diphenylamine, and then adding 400g of nitrocellulose to obtain a mixture;
a forming step: putting the mixture into equipment with a hole at the bottom and a vacuum at the lower part, pressurizing the top, and performing suction filtration below the equipment at the same time to obtain a solid material;
and (3) pelletizing: immersing the solid material into water, cutting into particles with the particle size of 95 meshes, and recovering the organic solvent in the water by using calcium chloride after cutting into particles;
the preparation method has no emulsification step.
8. A mono-based powder, characterized in that it is prepared by a process according to any one of claims 1 to 7.
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| US4694753A (en) * | 1986-02-26 | 1987-09-22 | Olin Corporation | Continuous production of low density base grain with a salt-free liquor |
| FR2930548A1 (en) * | 1992-02-12 | 2009-10-30 | Poudres & Explosifs Ste Nale | Double-base propellant composition having a high specific impulse and a significant plateau effect, and burning with a high combustion speed, obtained by molding a powder made of nitrocellulose with molding solvent |
| CN1176883C (en) * | 1999-02-08 | 2004-11-24 | 大连金州华日化工产品有限公司 | Method for preparing nitrocotton from single base propellant |
| CN101844954B (en) * | 2010-05-21 | 2012-06-27 | 南京理工大学 | Microporous smokeless firework explosive and preparation method thereof |
| CN103524278A (en) * | 2012-11-23 | 2014-01-22 | 周健 | Processing method of single-base powder and double-base powder for fireworks |
| CN104003825B (en) * | 2014-05-30 | 2016-08-24 | 泸州北方化学工业有限公司 | Wood pulp nitrocellulose single-base gun propellant and preparation method thereof |
| US20210147312A1 (en) * | 2017-06-23 | 2021-05-20 | Simmel Difesa S.P.A. | Composition for single-base propelling powder for ammunition and ammunition provided with such composition |
| CN109438146B (en) * | 2018-10-15 | 2021-05-04 | 北方化学工业股份有限公司 | Slurry production process of nitrocotton for indoor fireworks |
| CN109251116B (en) * | 2018-10-15 | 2021-04-23 | 北方化学工业股份有限公司 | Production method of nitrocotton for indoor fireworks |
| CN111362768A (en) * | 2018-12-26 | 2020-07-03 | 浏阳市景升烟花制造有限公司 | Smokeless bud-opening medicine |
| CN110540484B (en) * | 2019-10-14 | 2021-06-15 | 北方化学工业股份有限公司 | Continuous preparation process of nitrocotton for fireworks |
| CN111533814A (en) * | 2020-05-13 | 2020-08-14 | 张宏善 | Production process of nitrocotton and application of nitrocotton |
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