CN108586166A - A kind of method for coating of TKX-50 - Google Patents
A kind of method for coating of TKX-50 Download PDFInfo
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- CN108586166A CN108586166A CN201810418395.5A CN201810418395A CN108586166A CN 108586166 A CN108586166 A CN 108586166A CN 201810418395 A CN201810418395 A CN 201810418395A CN 108586166 A CN108586166 A CN 108586166A
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- tkx
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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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- Organic Chemistry (AREA)
- Paints Or Removers (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
- Application Of Or Painting With Fluid Materials (AREA)
Abstract
The present invention relates to the method for coating of TKX 50 a kind of, more particularly to 1,1' of one kind dihydroxy 5, the method for coating of 5' bistetrazole dihydroxy amine salt belongs to energetic material field.The present invention is used cooperatively using nitroguanidine and macromolecule, the best cladding realized to TKX 50 is created by technique, efficiently solve the problems, such as the cladding of 50 explosives of TKX, and preparation process is simple to operation, no complicated production device, preparation process is without high temperature pressure device, process conditions condition easily realizes that solvent for use and the repeatable recycling of glue meet environmental requirement, safe operation is reliable, it can be achieved that industrialized production.
Description
Technical field
The present invention relates to the method for coating of one kind 1,1'- dihydroxy -5,5'- bistetrazole dihydroxy amine salt (TKX-50), belong to
Energetic material field.
Background technology
TKX-50 is a kind of cage type novel high-energy explosive, white crystals graininess tetrazolium containing can ion salt, have high-energy,
Low sensitivity is the novel energetic material occurred in recent years, by global application field extensive concern.Numerous documents have recorded TKX-50
Synthetic technological condition optimization and formula theoretical calculation etc. report, but in insensitiveness and powder charge application aspect is few grinds
Study carefully document report.The rational surface cladding of single chmical compound explosive handles and does not influence explosion property, is explosive loading technology, and single
Can matter explosive realize the key using multiple link.Since the efficient coated explosive technology of James is announced, the explosive of early stage
Being passivated coating technology mainly also has composite material cladding process, passivation nitro compounds as the side such as deterrent cladding process, surfactant
Method.Wherein, the application of high polymer coated explosive is most, and effect is good.TKX-50 is a kind of salt energetic material, material it is compatible
Property etc. require high, it is poor directly to coat modifying interface effect using high polymer, and mechanical property and detonation property are all undesirable when powder charge；
Composite material, which coats TKX-50, has good foreground, there is no the phase for successfully utilizing this method successfully to coat TKX-50 so far
Close report；When surfactant coats TKX-50, the performance of the factors influences product such as type and dosage of surfactant.
Nitroguanidine (NQ) is a kind of white needle-like crystals that extremely low mechanical sensitivity is 0%, is the excellent blunt of energetic material
Agent, plane of crystal physical property is similar with TKX-50, both belongs to inorganic salts energetic material, has preferable compatible
Property, and have no document report in terms of cladding insensitiveness TKX-50 of the nitroguanidine with high molecular material cooperation for TKX-50 explosives.This
Invention is used cooperatively using nitroguanidine and macromolecule, is created the best cladding realized to TKX-50 by technique, is effectively solved
It has determined the cladding problems of TKX-50 explosives.
Invention content
It is an object of the present invention to provide a kind of method for coating of TKX-50, this method makes TKX-50 keep excellent detonation
While effect, and solves powder charge performance and improve its safety simultaneously.
The purpose of the present invention is what is be achieved through the following technical solutions.
A kind of method for coating of TKX-50, is as follows：
Step 1: at a temperature of 60~100 DEG C, after nitroguanidine in water stirring and dissolving, keeps temperature-resistant, be added
TKX-50, stirring 10~after sixty minutes, under static condition, solution temperature is dropped rapidly with 2~5 DEG C of cooling rate per minute
To 40~70 DEG C, solution is then down to 5~10 DEG C with 0.5~5 DEG C of cooling rate per minute, filtering obtains white product；
The additive amount of the nitroguanidine is the 0.5%~5% of TKX-50 mass；The quality of the water is 1~5 times of TKX-50 mass.
Step 2: by macromolecule dissolution to solvent, after being uniformly dissolved, the liquid that mass fraction is 0.7%~5% is obtained
Glue；
Step 3: the white product of gained in step 1 is added in the liquid glue obtained by step 2, stirs evenly, obtain
To mixed solution；The addition mass ratio of the white product and liquid glue is 4：(1~10)；
Step 4: lasting stirring, while the mixed solution into water L1 obtained by addition step 3, after addition, continue
Stirring 5~20 minutes；Stir speed (S.S.) is 200~700 revs/min；Then water L2 is added, is stirred evenly, filter and will be filtered
Products therefrom is 3~8 hours dry under being 380~490mmHg in 40~80 DEG C, vacuum degree, obtains the TKX-50 explosives coated.
The mass ratio of the mixed solution and L1 are 1：(5~20)；The mass ratio of the L1 and L2 is 1：(1~5)；
Macromolecule described in step 2 is one kind in fluorubber, silicon rubber, polystyrene or polymethyl methacrylate,
It is preferred that fluorubber, silicon rubber；
Solvent described in step 2 is one kind in ethyl acetate, tetrahydrofuran, ether or normal heptane；
Described in step 4 into water L1 be added step 3 obtained by mixed solution when, need to ensure to add in 10~60 minutes
It adds into.
Advantageous effect
1, the method for coating of a kind of TKX-50 of the invention, preparation process is simple to operation, no complicated production device, prepares
Process easily realizes that solvent for use and the repeatable recycling of glue meet environmental protection and want without high temperature pressure device, process conditions condition
It asks, safe operation is reliable, it can be achieved that industrialized production.
2, the method for coating of a kind of TKX-50 of the invention, product yield obtained is higher, after which is made cladding
The yield of TKX-50 is 99%~99.99%, and the grain graininess of gained can be evenly distributed on 20~80 mesh (Unite States Standard sieve) model
It encloses, mobility, press formability are good.
3, the method for coating of a kind of TKX-50 of the invention, products obtained therefrom covered effect is good, and friction is low with impact sensitivity,
Ensure not influencing its explosion property while security application.
Specific implementation mode
Present disclosure is described further in conjunction with the embodiments.
Embodiment 1
A kind of method for coating of TKX-50, is as follows：
At a temperature of 80 DEG C, by 1.5g nitroguanidines in 200g water after stirring and dissolving, keeps temperature-resistant, be added
Under static condition, 55 are rapidly decreased to 3 DEG C of cooling rate per minute after stirring 35 minutes by 98gTKX-50 for solution temperature
DEG C, solution is then down to 5 DEG C with 0.5 DEG C of cooling rate per minute, filtering obtains white product；0.5g fluorubber is molten
In solution to 50g ethyl acetate solvents, after being uniformly dissolved, the liquid glue that mass fraction is 0.99% is obtained；By the white production of gained
Object (99.3g) is added in 50.5g liquid glues, and stirring makes liquid glue form 149.8g homogeneous mixtures；149.8g is uniformly mixed
It closes object to be stirred with the rotating speed of 220r/min down in 750g water, after addition, continues after stirring 10min, add
750g water makes it be fully dispersed in water after continuing stirring 15 minutes, filters and the vacuum degree by filtration product at 45 DEG C is
Drying is taken out after 6 hours in the vacuum drying chamber of 410mmHg, obtains the TKX-50 explosive products coated.
TKX-50 white powders product 99.2g after being coated, yield 99.2%, it is 11% to hit explosion probability
(10kg drops hammer), characteristic drop height are 24cm (25kg drops hammer), and friction explosion probability is 20% (3.92MPa, 90 °), explosion velocity
9034m/s (ρ=1.803g/cm3)。
Embodiment 2
A kind of method for coating of TKX-50, is as follows：
At a temperature of 85 DEG C, by 12g nitroguanidines in 2000g water after stirring and dissolving, keeps temperature-resistant, be added
Solution temperature under static condition, is rapidly decreased to by 978gTKX-50 after stirring 25 minutes with 4 DEG C of cooling rate per minute
65 DEG C, solution is then down to 7 DEG C with 1 DEG C of cooling rate per minute, filtering obtains white product；10g silicon rubber is dissolved
Into 680g tetrahydrofuran solvents, after being uniformly dissolved, the liquid glue that mass fraction is 1.45% is obtained；By white product
(989.4g) is added in 690g liquid glues, stirring, and liquid glue is made to form the uniform gluing mixing jellies of 1679.4g；It will
1679.4g jellies are added in 8400g water, while being stirred with 250 revs/min of rotating speed, and addition finishes, and continue to stir
Dispersion 10 minutes is mixed, 8500g water is added, continues stirring after twenty minutes, filters and the vacuum degree by filtration product at 40 DEG C is
Drying is taken out after 8 hours in the vacuum drying chamber of 390mmHg, obtains the TKX-50 products coated.
TKX-50 white powders product 993g after being coated, yield 99.3%, shock explosion probability are 10% (10kg
Drop hammer), characteristic drop height is 27cm (25kg drops hammer), and friction explosion probability is 11% (3.92MPa, 90 °), explosion velocity 9049m/s (ρ
=1.813g/cm3)。
Embodiment 3
A kind of method for coating of TKX-50, is as follows：
At a temperature of 88 DEG C, by 1.7g nitroguanidines in 200g water after stirring and dissolving, keeps temperature-resistant, be added
Solution temperature under static condition, is rapidly decreased to by 96.8gTKX-50 after stirring 30 minutes with 5 DEG C of cooling rate per minute
60 DEG C, solution is then down to 8 DEG C with 1.5 DEG C of cooling rate per minute, filtering obtains white product；By 1.5g polyphenyl second
Alkene is dissolved into 50g ether solvents, after being uniformly dissolved, obtains the liquid glue that mass fraction is 2.9%；By white product
(98.1g) is added in 50g liquid glues, stirring, so that liquid glue is formed 149.6g and is uniformly mixed jelly；By 149.6g glues
Object is added in 850g water, while being stirred with 250r/min rotating speeds, and addition finishes, and after continuing stirring 15 minutes, is added
950g water, continue stirring 18 minutes, filter and by filtration product 50 DEG C vacuum degree be 440mmHg vacuum drying chamber in do
It is taken out after dry 5 hours, obtains the TKX-50 products coated.
TKX-50 white powders product 99.4g after being coated, yield 99.4%, shock explosion probability are 8% (10kg
Drop hammer), characteristic drop height is 28cm (25kg drops hammer), and friction explosion probability is 13% (3.92MPa, 90 °), explosion velocity 9021m/s (ρ
=1.798g/cm3)。
Embodiment 4
A kind of method for coating of TKX-50, is as follows：
At a temperature of 90 DEG C, by 3g nitroguanidines in 300g water after stirring and dissolving, keeps temperature-resistant, be added
Under static condition, 45 are rapidly decreased to 5 DEG C of cooling rate per minute after stirring 25 minutes by 96gTKX-50 for solution temperature
DEG C, solution is then down to 9 DEG C with 0.5 DEG C of cooling rate per minute, filtering obtains white product；By 1g polymethyls
Sour methyl esters is dissolved into 50g normal heptane solvents, after being uniformly dissolved, obtains the liquid glue that mass fraction is 1.96%；White is produced
Object (98.7g) is added in 51g liquid glues, stirring, so that liquid glue is formed 149.7g and is uniformly mixed jelly；By 149.7 mixing
Jelly is added into 780g water, while being stirred with 280 revs/min of rotating speed, and addition finishes, and continues stirring 20 minutes,
Add 800g water, continue stirring 20 minutes, filter and by filtration product 60 DEG C vacuum degree be 480mmHg vacuum drying
Drying is taken out after 4 hours in case, obtains the TKX-50 products coated.
TKX-50 white powders product 99.6g after being coated, yield 99.6%, shock explosion probability are 7% (10kg
Drop hammer), characteristic drop height be 22cm (25kg drops hammer), friction explosion probability be 8% (3.92MPa, 90 °), explosion velocity 9019m/s (ρ=
1.795g/cm3)。
Above-described specific descriptions have carried out further specifically the purpose, technical solution and advantageous effect of invention
It is bright, it should be understood that the above is only a specific embodiment of the present invention, the protection model being not intended to limit the present invention
It encloses, all within the spirits and principles of the present invention, any modification, equivalent substitution, improvement and etc. done should be included in the present invention
Protection domain within.
Claims (5)
1. a kind of method for coating of TKX-50, it is characterised in that：It is as follows：
Step 1: at a temperature of 60~100 DEG C, after nitroguanidine in water stirring and dissolving, keeps temperature-resistant, TKX- is added
50, stirring 10~after sixty minutes, under static condition, solution temperature is rapidly decreased to 40 with 2~5 DEG C of cooling rate per minute
~70 DEG C, solution is then down to 5~10 DEG C with 0.5~5 DEG C of cooling rate per minute, white product is obtained after filtering；Institute
The additive amount for stating nitroguanidine is the 0.5%~5% of TKX-50 mass；The quality of the water is 1~5 times of TKX-50 mass；
Step 2: by macromolecule dissolution to solvent, after being uniformly dissolved, the liquid glue that mass concentration is 0.7%~5% is obtained；
Step 3: the white product of gained in step 1 is added in the liquid glue obtained by step 2, stirs evenly, mixed
Close solution；The addition mass ratio of the white product and liquid glue is 4：(1~10)；
Step 4: lasting stirring, while the mixed solution into water L1 obtained by addition step 3, after addition, continue stirring 5
~20 minutes；Stir speed (S.S.) is 200~700 revs/min；Then water L2 is added, is stirred evenly, filter and produces filtering gained
Object is 3~8 hours dry under being 380~490mmHg in 40~80 DEG C, vacuum degree, obtains the TKX-50 explosives coated；It is described mixed
The mass ratio for closing solution and L1 is 1：(5~20)；The mass ratio of the L1 and L2 is 1：(1~5).
2. a kind of method for coating of TKX-50 as described in claim 1, it is characterised in that：Macromolecule described in step 2 is fluorine
One kind in rubber, silicon rubber, polystyrene or polymethyl methacrylate.
3. a kind of method for coating of TKX-50 as claimed in claim 2, it is characterised in that：It is fluorine that the macromolecule, which is preferentially selected,
Rubber or silicon rubber.
4. a kind of method for coating of TKX-50 as described in claim 1, it is characterised in that：Solvent described in step 2 is acetic acid
Ethyl ester, tetrahydrofuran, ether or normal heptane.
5. a kind of method for coating of TKX-50 as described in claim 1, it is characterised in that：It is added into water L1 described in step 4
When mixed solution obtained by step 3, it need to ensure finishing in the addition of 10~60 minutes.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810418395.5A CN108586166B (en) | 2018-05-04 | 2018-05-04 | TKX-50 coating method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810418395.5A CN108586166B (en) | 2018-05-04 | 2018-05-04 | TKX-50 coating method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN108586166A true CN108586166A (en) | 2018-09-28 |
| CN108586166B CN108586166B (en) | 2020-09-18 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810418395.5A Active CN108586166B (en) | 2018-05-04 | 2018-05-04 | TKX-50 coating method |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106083495A (en) * | 2016-06-17 | 2016-11-09 | 中国工程物理研究院化工材料研究所 | Coated explosive microsphere that the solidification of a kind of emulsion prepares and preparation method thereof |
| 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 |
-
2018
- 2018-05-04 CN CN201810418395.5A patent/CN108586166B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN106083495A (en) * | 2016-06-17 | 2016-11-09 | 中国工程物理研究院化工材料研究所 | Coated explosive microsphere that the solidification of a kind of emulsion prepares and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| JUNFENG WANG等: "《Preparation, Characterization, Thermal Evaluation and Sensitivities of TKX-50/GO Composite》", 《PROPELLANTS,EXPLOSIVES,PYROTECHNICS》 * |
| 苗成才等: "《新型联四唑类含能材料TKX– 50 的研究进展》", 《化学推进剂与高分子材料》 * |
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| CN108586166B (en) | 2020-09-18 |
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