CN108586166B - TKX-50 coating method - Google Patents
TKX-50 coating method Download PDFInfo
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- CN108586166B CN108586166B CN201810418395.5A CN201810418395A CN108586166B CN 108586166 B CN108586166 B CN 108586166B CN 201810418395 A CN201810418395 A CN 201810418395A CN 108586166 B CN108586166 B CN 108586166B
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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
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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
- C06B25/34—Compositions containing a nitrated organic compound the compound being a nitrated acyclic, alicyclic or heterocyclic amine
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- Paints Or Removers (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
- Application Of Or Painting With Fluid Materials (AREA)
Abstract
The invention relates to a TKX-50 coating method, in particular to a coating method of 1, 1 '-dihydroxy-5, 5' -bitetrazole dihydroxylamine, belonging to the field of energetic materials. The invention utilizes the cooperation of nitroguanidine and macromolecule for use, realizes the optimal coating of TKX-50 through the process creation, effectively solves the coating problem of TKX-50 explosive, has simple and easy operation of preparation process, no complex production device, no high-temperature pressure device in the preparation process, easy realization of process condition conditions, repeated recycling of used solvent and glue solution, conforms to the environmental protection requirement, safe and reliable operation and can realize industrial production.
Description
Technical Field
The invention relates to a coating method of 1, 1 '-dihydroxy-5, 5' -bistetrazole dihydroxylamine (TKX-50), belonging to the field of energetic materials.
Background
TKX-50 is a novel cage-shaped high-energy explosive, white crystalline granular tetrazole energetic ion salt, a novel energetic material with high energy and low sensitivity appears in recent years, and the novel energetic material is widely concerned by the global application field. A plurality of literatures record reports on optimization of synthesis process conditions, theoretical calculation of a formula and the like of TKX-50, but few research documents report on insensitive and charging application. The reasonable surface coating treatment of the single-substance explosive does not influence the explosive property, is an explosive charging technology and is a key for realizing multiple links of application of the single-substance explosive. Since the publication of the James' high-efficiency explosive coating technology, the early explosive passivation coating technology mainly comprises a composite material coating method, a passivation nitro-compound serving as a desensitizer coating method, a surfactant and the like. Wherein, the application of the high polymer coated explosive is the most, and the effect is good. TKX-50 is a salt energetic material, the requirements on compatibility and the like of the material are high, the interface is directly coated by a high polymer, the modification effect is poor, and the mechanical property and the detonation property are not ideal during charging; the TKX-50 coated by the composite material has good prospect, and no related report that the TKX-50 is successfully coated by the method exists so far; when the TKX-50 is coated by the surfactant, the performance of the product is influenced by factors such as the type and the dosage of the surfactant.
Nitroguanidine (NQ) is a white needle crystal with extremely low mechanical sensitivity of 0 percent, is an excellent passivator for energetic materials, has crystal surface physical properties similar to those of TKX-50, both belong to inorganic salt energetic materials and have good compatibility, and the nitroguanidine and a high polymer material are matched for coating the insensitive TKX-50 of the TKX-50 explosive and are not reported in documents. The invention utilizes the cooperation of nitroguanidine and macromolecules, realizes the optimal coating of TKX-50 through the process creation, and effectively solves the coating problem of TKX-50 explosives.
Disclosure of Invention
The invention aims to provide a method for coating TKX-50, which ensures that the TKX-50 maintains excellent detonation effect, solves the problem of explosive charging performance and improves the safety of the TKX-50.
The purpose of the invention is realized by the following technical scheme.
A method for coating TKX-50 comprises the following specific steps:
step one, stirring and dissolving nitroguanidine in water at the temperature of 60-100 ℃, keeping the temperature unchanged, adding TKX-50, stirring for 10-60 minutes, rapidly cooling the solution to 40-70 ℃ at the cooling speed of 2-5 ℃ per minute in a standing state, then cooling the solution to 5-10 ℃ at the cooling speed of 0.5-5 ℃ per minute, and filtering to obtain a white product; the addition amount of the nitroguanidine is 0.5-5% of the mass of TKX-50; the mass of the water is 1-5 times of that of the TKX-50.
Step two, dissolving the polymer into a solvent, and obtaining a liquid glue with the mass fraction of 0.7-5% after uniform dissolution;
step three, adding the white product obtained in the step one into the liquid glue obtained in the step two, and uniformly stirring to obtain a mixed solution; the adding mass ratio of the white product to the liquid glue is 4: (1-10);
step four, continuously stirring, adding the mixed solution obtained in the step three into water L1, and continuously stirring for 5-20 minutes after the addition is finished; the stirring speed is 200-700 r/min; and then adding water L2, stirring uniformly, filtering, and drying the filtered product at 40-80 ℃ under the vacuum degree of 380-490 mmHg for 3-8 hours to obtain the coated TKX-50 explosive. The mass ratio of the mixed solution to the L1 is 1: (5-20); the mass ratio of the L1 to the L2 is 1: (1-5);
in the second step, the polymer is one of fluororubber, silicon rubber, polystyrene or polymethyl methacrylate, preferably fluororubber and silicon rubber;
in the second step, the solvent is one of ethyl acetate, tetrahydrofuran, diethyl ether or n-heptane;
and step four, when the mixed solution obtained in the step three is added into the water L1, the addition is ensured to be completed within 10-60 minutes.
Advantageous effects
1. The TKX-50 coating method has the advantages of simple and easy operation of preparation process, no complex production device, no high-temperature pressure device in the preparation process, easy realization of process condition, repeated recycling of used solvent and glue solution, environmental protection requirement conformity, safe and reliable operation and realization of industrial production.
2. The TKX-50 coating method provided by the invention has the advantages that the yield of the prepared product is high, the yield of the TKX-50 coated by the product is 99% -99.99%, the particle size of the obtained particles can be uniformly distributed in the range of 20-80 meshes (American standard sieve), and the mobility and the press formability are good.
3. The TKX-50 coating method provided by the invention has the advantages that the obtained product is good in coating effect and low in friction and impact sensitivity, and the explosion performance of the TKX-50 coating method is not influenced while the safe application is ensured.
Detailed Description
The present invention will be further described with reference to examples.
Example 1
A method for coating TKX-50 comprises the following specific steps:
stirring 1.5g of nitroguanidine in 200g of water at the temperature of 80 ℃ to dissolve, keeping the temperature constant, adding 98g of TKX-50, stirring for 35 minutes, rapidly cooling the solution to 55 ℃ at the cooling rate of 3 ℃ per minute in a standing state, then cooling the solution to 5 ℃ at the cooling rate of 0.5 ℃ per minute, and filtering to obtain a white product; dissolving 0.5g of fluororubber into 50g of ethyl acetate solvent, and obtaining liquid rubber with the mass fraction of 0.99% after uniform dissolution; the resulting white product (99.3g) was added to 50.5g of liquid gum and stirred to form 149.8g of a homogeneous mixture; pouring 149.8g of the uniform mixture into 750g of water, stirring at the rotating speed of 220r/min, continuing to stir for 10min after the addition is finished, then adding 750g of water, continuing to stir for 15 min, completely dispersing the mixture into the water, filtering, drying the filtered product in a vacuum drying oven with the vacuum degree of 410mmHg at 45 ℃ for 6 hours, and taking out the dried product to obtain the coated TKX-50 explosive product.
99.2g of the coated TKX-50 white powder product is obtained, the yield is 99.2%, the collision and explosion probability is 11% (10kg drop weight), the characteristic drop height is 24cm (25kg drop weight), the friction and explosion probability is 20% (3.92MPa, 90 degrees), and the explosion speed is 9034m/s (rho is 1.803 g/cm)3)。
Example 2
A method for coating TKX-50 comprises the following specific steps:
stirring 12g of nitroguanidine in 2000g of water at 85 ℃ to dissolve, keeping the temperature constant, adding 978g of TKX-50, stirring for 25 minutes, rapidly cooling the solution to 65 ℃ at a cooling rate of 4 ℃ per minute in a standing state, then cooling the solution to 7 ℃ at a cooling rate of 1 ℃ per minute, and filtering to obtain a white product; dissolving 10g of silicon rubber into 680g of tetrahydrofuran solvent, and obtaining liquid rubber with the mass fraction of 1.45% after uniform dissolution; the white product (989.4g) was added to 690g of liquid gum and stirred to form 1679.4g of a homogeneous viscous mixed gum; 1679.4g of jelly is added into 8400g of water, the stirring is carried out at the rotating speed of 250 rpm, after the addition is finished, the stirring and the dispersion are continued for 10 minutes, 8500g of water is added, the stirring is continued for 20 minutes, the filtration is carried out, and the filtered product is dried in a vacuum drying oven with the vacuum degree of 390mmHg at 40 ℃ for 8 hours and then taken out, so that the coated TKX-50 product is obtained.
993g of the coated TKX-50 white powder product is obtained, the yield is 99.3%, the collision and explosion probability is 10% (10kg drop weight), the characteristic drop height is 27cm (25kg drop weight), the friction and explosion probability is 11% (3.92MPa, 90 degrees), and the explosion speed is 9049m/s (rho is 1.813 g/cm)3)。
Example 3
A method for coating TKX-50 comprises the following specific steps:
stirring 1.7g of nitroguanidine in 200g of water at the temperature of 88 ℃ to dissolve, keeping the temperature constant, adding 96.8g of TKX-50, stirring for 30 minutes, rapidly cooling the solution to 60 ℃ at the cooling rate of 5 ℃ per minute in a standing state, then cooling the solution to 8 ℃ at the cooling rate of 1.5 ℃ per minute, and filtering to obtain a white product; dissolving 1.5g of polystyrene into 50g of ether solvent, and obtaining a liquid glue with the mass fraction of 2.9% after uniform dissolution; the white product (98.1g) was added to 50g of liquid gum and stirred to form 149.6g of a homogeneous mixed gum; and adding 149.6g of the jelly into 850g of water, stirring at the speed of 250r/min, continuing to stir for 15 minutes after the addition is finished, adding 950g of water, continuing to stir for 18 minutes, filtering, drying the filtered product in a vacuum drying oven with the vacuum degree of 440mmHg at 50 ℃ for 5 hours, and taking out to obtain the coated TKX-50 product.
99.4g of the coated TKX-50 white powder product is obtained, the yield is 99.4%, the collision and explosion probability is 8% (10kg drop weight), the characteristic drop height is 28cm (25kg drop weight), the friction and explosion probability is 13% (3.92MPa, 90 degrees), and the explosion speed is 9021m/s (rho is 1.798 g/cm)3)。
Example 4
A method for coating TKX-50 comprises the following specific steps:
stirring 3g of nitroguanidine in 300g of water at the temperature of 90 ℃ to dissolve, keeping the temperature constant, adding 96g of TKX-50, stirring for 25 minutes, rapidly cooling the solution to 45 ℃ at the cooling rate of 5 ℃ per minute in a standing state, then cooling the solution to 9 ℃ at the cooling rate of 0.5 ℃ per minute, and filtering to obtain a white product; dissolving 1g of polymethyl methacrylate into 50g of n-heptane solvent, and obtaining a liquid adhesive with the mass fraction of 1.96% after uniform dissolution; the white product (98.7g) was added to 51g of liquid gum and stirred to form 149.7g of a homogeneous mixed gum; adding the 149.7 mixed jelly into 780g of water, stirring at the speed of 280 revolutions per minute, continuing to stir for 20 minutes after the addition is finished, adding 800g of water, continuing to stir for 20 minutes, filtering, drying the filtered product in a vacuum drying oven with the vacuum degree of 480mmHg at 60 ℃ for 4 hours, and taking out to obtain the coated TKX-50 product.
99.6g of the coated TKX-50 white powder product is obtained, the yield is 99.6%, the collision and explosion probability is 7% (10kg drop weight), the characteristic drop height is 22cm (25kg drop weight), the friction and explosion probability is 8% (3.92MPa, 90 degrees), and the explosion speed is 9019m/s (rho is 1.795 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 and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (5)
1. A TKX-50 coating method is characterized in that: the method comprises the following specific steps:
step one, stirring and dissolving nitroguanidine in water at the temperature of 60-100 ℃, keeping the temperature unchanged, adding TKX-50, stirring for 10-60 minutes, rapidly cooling the solution to 40-70 ℃ at the cooling speed of 2-5 ℃ per minute in a standing state, then cooling the solution to 5-10 ℃ at the cooling speed of 0.5-5 ℃ per minute, and filtering to obtain a white product; the addition amount of the nitroguanidine is 0.5-5% of the mass of TKX-50; the mass of the water is 1-5 times of that of the TKX-50;
step two, dissolving the macromolecule into a solvent, and obtaining liquid glue with the mass concentration of 0.7-5% after uniform dissolution;
step three, adding the white product obtained in the step one into the liquid glue obtained in the step two, and uniformly stirring to obtain a mixed solution; the adding mass ratio of the white product to the liquid glue is 4: (1-10);
step four, continuously stirring, adding the mixed solution obtained in the step three into water L1, and continuously stirring for 5-20 minutes after the addition is finished; the stirring speed is 200-700 r/min; then adding water L2, stirring uniformly, filtering, and drying the filtered product at 40-80 ℃ under the vacuum degree of 380-490 mmHg for 3-8 hours to obtain the coated TKX-50 explosive; the mass ratio of the mixed solution to the L1 is 1: (5-20); the mass ratio of the L1 to the L2 is 1: (1-5).
2. The method for coating TKX-50 of claim 1, wherein: in the second step, the polymer is one of fluororubber, silicone rubber, polystyrene or polymethyl methacrylate.
3. The method for coating TKX-50 of claim 2, wherein: the polymer is preferably a fluorine rubber or a silicon rubber.
4. The method for coating TKX-50 of claim 1, wherein: and in the second step, the solvent is ethyl acetate, tetrahydrofuran, diethyl ether or n-heptane.
5. The method for coating TKX-50 of claim 1, wherein: and step four, when the mixed solution obtained in the step three is added into the water L1, the addition is ensured to be finished within 10-60 minutes.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810418395.5A CN108586166B (en) | 2018-05-04 | 2018-05-04 | TKX-50 coating method |
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| CN201810418395.5A CN108586166B (en) | 2018-05-04 | 2018-05-04 | TKX-50 coating method |
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| CN108586166B true CN108586166B (en) | 2020-09-18 |
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| 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 |
| CN106083495B (en) * | 2016-06-17 | 2018-02-06 | 中国工程物理研究院化工材料研究所 | Coated explosive microballoon that a kind of emulsion solidification is prepared and preparation method thereof |
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