CN108558587B - Method for coating TKX-50 by nitroguanidine through fluidization, spray granulation - Google Patents
Method for coating TKX-50 by nitroguanidine through fluidization, spray granulation Download PDFInfo
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- CN108558587B CN108558587B CN201810418676.0A CN201810418676A CN108558587B CN 108558587 B CN108558587 B CN 108558587B CN 201810418676 A CN201810418676 A CN 201810418676A CN 108558587 B CN108558587 B CN 108558587B
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- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
- C06B23/00—Compositions characterised by non-explosive or non-thermic constituents
- C06B23/005—Desensitisers, phlegmatisers
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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
- C06B21/00—Apparatus or methods for working-up explosives, e.g. forming, cutting, drying
- C06B21/0083—Treatment of solid structures, e.g. for coating or impregnating with a modifier
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- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
- C06B45/00—Compositions or products which are defined by structure or arrangement of component of product
- C06B45/18—Compositions or products which are defined by structure or arrangement of component of product comprising a coated component
- C06B45/20—Compositions or products which are defined by structure or arrangement of component of product comprising a coated component the component base containing an organic explosive or an organic thermic component
- C06B45/22—Compositions or products which are defined by structure or arrangement of component of product comprising a coated component the component base containing an organic explosive or an organic thermic component the coating containing an organic compound
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- Organic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Glanulating (AREA)
- Application Of Or Painting With Fluid Materials (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
Abstract
The invention relates to a method for coating TKX-50 by nitroguanidine fluidization, spray granulation, and belongs to the field of energetic materials. The method comprises the following steps: adding polyvinyl butyral into ethyl acetate, keeping the temperature unchanged, and stirring to completely dissolve the polyvinyl butyral to obtain a liquid glue; adding nitroguanidine into the liquid gum at 50 ℃, and stirring to completely dissolve the nitroguanidine to obtain the nitroguanidine-containing liquid gum; adding TKX-50 into a fluidized bed granulating device at the temperature of 35 ℃, continuously mixing for 40min, spraying nitroguanidine-containing liquid glue into a fluidized layer of the fluidized bed granulating device, mixing and granulating, drying in the fluidized bed granulating device at the temperature of 40 ℃, and sieving to obtain the TKX-50 coated with nitroguanidine granules; the preparation process is simple, a high-temperature pressurizing and depressurizing device is not needed in the preparation process, and the used solvent can be recycled. The product yield is high, the yield of the TKX-50 coated by the fluidized spray granulation is 99-99.99%, and the obtained particles are uniform in particle size and good in flowability and press formability.
Description
Technical Field
The invention relates to a method for coating TKX-50 by nitroguanidine fluidization, spray granulation, and belongs to the field of energetic materials.
Background
The requirement of high-efficiency damage on the explosive power performance is continuously improved, and the energetic material required by the modern weapon system has the characteristics of high energy density, low vulnerability, high safety and the like. 1, 1 '-dihydroxy-5, 5' -bistetrazole dihydroxylamine (hereinafter TKX-50) is a novel high-energy elementary explosive, is a white crystalline granular high-energy low-sensitivity tetrazole energetic ion salt, is a novel energetic material appearing in recent years, and is widely concerned in the application field due to high energy. The majority of the mixed explosive literature does not discover mixed explosives related to TKX-50, and the literature is common in terms of optimization of synthesis process conditions of TKX-50 and theoretical calculation of formula. The insensitive coating material of the TKX-50 not only influences the explosive property of the mixed explosive, but also influences the compatibility of the explosive, and the explosive property and the mechanical property of the TKX-50 coated by the existing method do not meet the requirements of an application department. The explosive passivation coating technology mainly comprises a high molecular polymer coating method, a composite material coating method, a passivation nitro-compound as a passivation agent coating method, a surfactant and the like. The effect of the composite material coated explosive is superior to that of other technologies, and the high-quality high-grade mixed explosive has high requirements on the compatibility of the material and the performance influence of the composite material on the explosive.
Nitroguanidine (NQ) is a white needle crystal with extremely low mechanical sensitivity of 0 percent, can be used as a mixed explosive passivator, but is not reported in documents on the aspect of insensitive TKX-50. The invention uses nitroguanidine to fluidize, spray and granulate to coat TKX-50. In the course of fluidization spray granulation, the material powder is kept in the suspended fluidized state under the action of air flow from bottom to top in the container, the liquid adhesive is sprayed into fluidized layer to make powder be coalesced into granules, and the 3 steps of mixing, granulating and drying are completed in a closed container at one time, and the whole course of granulation is not affected by external force, and only affected by air flow in the bed, so that the density of the prepared granules is small, and its strength is low, and the obtained granules are uniform in grain size, and good in flowability and compression formability.
Disclosure of Invention
The invention aims to provide a method for coating TKX-50 by nitroguanidine fluidization spray granulation, which can reduce the sensitivity of TKX-50, improve the charging performance, improve the charging safety and charging forming without influencing the energy level.
The purpose of the invention is realized by the following technical scheme.
A method for coating TKX-50 by nitroguanidine through fluidization, spray granulation comprises the following specific steps:
step one, adding an adhesive into an anhydrous solvent at the temperature of 20-70 ℃ and the stirring speed of 150-300 r/min, keeping the temperature unchanged, and stirring until the adhesive is completely dissolved to obtain a liquid adhesive with the mass fraction of 0.5-0.8%;
step two, adding nitroguanidine into the liquid glue prepared in the step one, and stirring at a stirring speed of 100-200 r/min at 40-50 ℃ to completely dissolve the nitroguanidine to obtain the liquid glue containing nitroguanidine;
step three, adding TKX-50 into a fluidized bed granulation device at the temperature of 15-35 ℃, continuously mixing for 20-40 min, spraying the liquid glue containing nitroguanidine obtained in the step two into a fluidized layer of the fluidized bed granulation device, and carrying out mixed granulation for 20-50 min to obtain a coated TKX-50 crude product;
sieving the coated TKX-50 crude product obtained in the step three, drying at the temperature of 15-60 ℃ for 2-8 h, and then granulating to obtain the TKX-50 coated with granulated nitroguanidine;
the addition mass ratio of the adhesive, nitroguanidine and TKX-50 is (0.5-1.5): (1-10): 100, respectively;
in the first step, the adhesive is one of polyvinyl butyral, polyacrylic acid, polymethyl acrylate and polymethyl methacrylate;
in the step one, the anhydrous solvent is any one of ethyl acetate, acetone and ethanol;
in the third step, the particle size of the TKX-50 is 100-300 meshes;
in the fourth step, the sieved grain size is 100-300 meshes.
Advantageous effects
1. The method for coating TKX-50 by nitroguanidine fluidization, spray granulation has the advantages of simple production and preparation device, simple preparation process and operation, no high-temperature pressurizing and depressurizing device in the preparation process, capability of repeatedly recycling the used solvent, accordance with the environmental protection requirement, safety and reliability in operation and capability of realizing industrial production.
2. The method for coating TKX-50 by nitroguanidine through fluidization, spray granulation and the like has the advantages that the yield of the prepared product is high, the yield of the TKX-50 coated by the nitroguanidine through fluidization, spray granulation and the like is 99-99.99%, and the obtained particles are uniform in particle size and good in flowability and press formability.
3. The method for coating TKX-50 by adopting fluidized spray granulation of nitroguanidine has the advantages that the obtained product is low in friction and impact sensitivity, and the energy level of the product is not influenced.
Detailed Description
The present invention will be further described with reference to examples.
Example 1
Adding 5g of polyvinyl butyral into 800g of ethyl acetate at 70 ℃ and a stirring speed of 300r/min, keeping the temperature unchanged, and stirring to completely dissolve the polyvinyl butyral to obtain a liquid glue with the mass fraction of 0.62%; adding 50g of nitroguanidine into the liquid gum at the temperature of 50 ℃ and at the stirring speed of 200r/min, and stirring to completely dissolve the nitroguanidine to obtain the nitroguanidine-containing liquid gum; adding 945gTKX-50 with the particle size of 230 meshes into a fluidized bed granulating device at the temperature of 35 ℃, continuously mixing for 40min, spraying the liquid glue containing nitroguanidine into a fluidized layer of the fluidized bed granulating device, mixing and granulating for 50min, drying for 4h in the fluidized bed granulating device at the temperature of 40 ℃, and sieving by using a 200-mesh sieve to obtain the TKX-50 coated with the nitroguanidine granules;
991g of TKX-50 white particle product after nitroguanidine granulation and coating is obtained, the yield is 99.1%, the impact explosion probability is 10% (10kg drop weight), the characteristic drop height is 22cm (25kg drop weight), the friction explosion probability is 9% (3.92M Pa, 90 degrees), and the explosion speed is 9045M/s (rho is 1.811 g/cm)3)。
Example 2
Adding 0.6g of polymethyl acrylate into 80g of ethanol at the temperature of 55 ℃ and the stirring speed of 200r/min, keeping the temperature unchanged, and stirring to completely dissolve the polymethyl acrylate to obtain a liquid adhesive with the mass fraction of 0.74%; adding 5g of nitroguanidine into 80g of liquid gum under the conditions of 45 ℃ and stirring speed of 180r/min, and stirring to completely dissolve the nitroguanidine to obtain liquid gum containing nitroguanidine; adding 94.4g of TKX-50 with the particle size of 200 meshes into a fluidized bed granulating device at the temperature of 30 ℃, continuously mixing for 35min, spraying liquid glue containing nitroguanidine into a fluidized layer of the fluidized bed granulating device, mixing and granulating for 40min, drying for 2h in the fluidized bed granulating device at the temperature of 50 ℃, and sieving by using a 230-mesh sieve to obtain the TKX-50 coated with the nitroguanidine granules;
99.4g of TKX-50 white granular product coated with nitroguanidine granules is obtained, the yield is 99.4%, the impact explosion probability is 10% (10kg drop weight), the characteristic drop height is 23cm (25kg drop weight), the friction explosion probability is 7% (3.92M Pa, 90 degrees), and the explosion speed is 9021M/s (rho is 1.806 g/cm)3)。
Example 3
Adding 0.5g of polyacrylic acid into 75g of ethanol at the temperature of 60 ℃ and the stirring speed of 190r/min, keeping the temperature unchanged, and stirring to completely dissolve the polyacrylic acid to obtain liquid glue with the mass fraction of 0.66%; adding 5.5g of nitroguanidine into 75g of liquid gum under the conditions of 40 ℃ and stirring speed of 180r/min, and stirring to completely dissolve the nitroguanidine to obtain liquid gum containing nitroguanidine; adding 94 g of TKX-50 with the particle size of 260 meshes into a fluidized bed granulation device at the temperature of 35 ℃, continuously mixing for 35min, spraying liquid glue containing nitroguanidine into a fluidized layer of the fluidized bed granulation device, mixing and granulating for 40min, drying for 8h in the fluidized bed granulation device at the temperature of 15 ℃, and sieving by using a 200-mesh sieve to obtain the TKX-50 coated with the nitroguanidine granules;
99.3g of TKX-50 white granular product coated with nitroguanidine granules is obtained, the yield is 99.3%, the impact explosion probability is 9% (10kg drop weight), the characteristic drop height is 21cm (25kg drop weight), the friction explosion probability is 8% (3.92M Pa, 90 degrees), and the explosion speed is 9048M/s (rho is 1.812 g/cm)3)。
Example 4
Adding 0.7g of polymethyl methacrylate into 90g of acetone at the temperature of 65 ℃ and the stirring speed of 180r/min, keeping the temperature unchanged, and stirring to completely dissolve the polymethyl methacrylate to obtain liquid glue with the mass fraction of 0.77%; adding 7g of nitroguanidine into 75g of liquid gum under the conditions of 48 ℃ and 175r/min of stirring speed, and stirring to completely dissolve the nitroguanidine to obtain liquid gum containing nitroguanidine; adding 92.3 g of TKX-50 with the particle size of 260 meshes into a fluidized bed granulating device at the temperature of 25 ℃, continuously mixing for 30min, spraying liquid glue containing nitroguanidine into a fluidized layer of the fluidized bed granulating device, mixing and granulating for 45min, drying for 3h in the fluidized bed granulating device at the temperature of 50 ℃, and sieving by using a 200-mesh sieve to obtain the TKX-50 coated with the nitroguanidine granules;
99.4g of TKX-50 white granular product coated with nitroguanidine granules is obtained, the yield is 99.4%, the impact explosion probability is 12% (10kg drop weight), the characteristic drop height is 24cm (25kg drop weight), the friction explosion probability is 6% (3.92M Pa, 90 degrees), and the explosion speed is 9037M/s (rho is 1.809 g/cm)3)。
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, etc. made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (4)
1. A method for coating TKX-50 by nitroguanidine fluidization and spray granulation is characterized in that: the method comprises the following specific steps:
step one, adding an adhesive into an anhydrous solvent at the temperature of 20-70 ℃ and the stirring speed of 150-300 r/min, keeping the temperature unchanged, stirring until the adhesive is completely dissolved to obtain a liquid adhesive with the mass fraction of 0.5-0.8%, and placing the liquid adhesive at the temperature of 20-50 ℃ for later use;
step two, adding nitroguanidine into the liquid glue prepared in the step one, and stirring at a stirring speed of 100-200 r/min at 40-50 ℃ to completely dissolve the nitroguanidine to obtain the liquid glue containing nitroguanidine;
step three, adding TKX-50 into a fluidized bed granulation device at the temperature of 15-35 ℃, continuously mixing for 20-40 min, spraying the liquid glue containing nitroguanidine obtained in the step two into a fluidized layer of the fluidized bed granulation device, and carrying out mixed granulation for 20-50 min to obtain a coated TKX-50 crude product;
sieving the coated TKX-50 crude product obtained in the step three, drying at the temperature of 15-60 ℃ for 2-8 h, and then granulating to obtain the TKX-50 coated with granulated nitroguanidine;
the addition mass ratio of the adhesive, nitroguanidine and TKX-50 is (0.5-1.5): (1-10): 100, respectively;
in the first step, the adhesive is one of polyvinyl butyral, polyacrylic acid, polymethyl acrylate and polymethyl methacrylate.
2. The method for fluidized spray granulation coating of TKX-50 by nitroguanidine as claimed in claim 1, wherein: in the step one, the anhydrous solvent is any one of ethyl acetate, acetone and ethanol.
3. The method for fluidized spray granulation coating of TKX-50 by nitroguanidine as claimed in claim 1, wherein: in the third step, the particle size of the TKX-50 is 100-300 meshes.
4. The method for fluidized spray granulation coating of TKX-50 by nitroguanidine as claimed in claim 1, wherein: in the fourth step, the sieved grain size is 100-300 meshes.
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| CN201810418676.0A CN108558587B (en) | 2018-05-04 | 2018-05-04 | Method for coating TKX-50 by nitroguanidine through fluidization, spray granulation |
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| CN201810418676.0A CN108558587B (en) | 2018-05-04 | 2018-05-04 | Method for coating TKX-50 by nitroguanidine through fluidization, spray granulation |
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| CN108558587B true CN108558587B (en) | 2020-09-18 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1405126A (en) * | 2002-11-13 | 2003-03-26 | 王志华 | Method for enhancing explosion property of explosive |
| CN103524444A (en) * | 2013-09-27 | 2014-01-22 | 北京理工大学 | Synthetic method of 5, 5'-bistetrazole-1, 1'-dioxo hydroxyl ammonium salt (TKX-50) |
| US9643937B1 (en) * | 2016-03-31 | 2017-05-09 | The United States Of America As Represented By The Secretary Of The Army | One-pot process for preparation of ammonium and hydroxyl ammonium derivatives of bis 5,5′-tetrazole-1,1′-dihydroxide |
| CN107879867A (en) * | 2017-06-28 | 2018-04-06 | 湖北航天化学技术研究所 | A kind of high-energy insensitive is pressed plastic bonded explosive |
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- 2018-05-04 CN CN201810418676.0A patent/CN108558587B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1405126A (en) * | 2002-11-13 | 2003-03-26 | 王志华 | Method for enhancing explosion property of explosive |
| CN103524444A (en) * | 2013-09-27 | 2014-01-22 | 北京理工大学 | Synthetic method of 5, 5'-bistetrazole-1, 1'-dioxo hydroxyl ammonium salt (TKX-50) |
| US9643937B1 (en) * | 2016-03-31 | 2017-05-09 | The United States Of America As Represented By The Secretary Of The Army | One-pot process for preparation of ammonium and hydroxyl ammonium derivatives of bis 5,5′-tetrazole-1,1′-dihydroxide |
| CN107879867A (en) * | 2017-06-28 | 2018-04-06 | 湖北航天化学技术研究所 | A kind of high-energy insensitive is pressed plastic bonded explosive |
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