CN108558587A - A kind of method that nitroguanidine fluidization spray is granulated cladding TKX-50 - Google Patents
A kind of method that nitroguanidine fluidization spray is granulated cladding TKX-50 Download PDFInfo
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- CN108558587A CN108558587A CN201810418676.0A CN201810418676A CN108558587A CN 108558587 A CN108558587 A CN 108558587A CN 201810418676 A CN201810418676 A CN 201810418676A CN 108558587 A CN108558587 A CN 108558587A
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- Prior art keywords
- tkx
- nitroguanidine
- cladding
- granulated
- liquid glue
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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
-
- 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
-
- 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
-
- 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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- Chemical & Material Sciences (AREA)
- 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 present invention relates to a kind of methods that nitroguanidine fluidization spray is granulated cladding TKX 50, belong to energetic material field.Method is：Polyvinyl butyral is added in ethyl acetate, keeps temperature-resistant, stirring makes it completely dissolved, and obtains liquid glue；At 50 DEG C, nitroguanidine is added in aforesaid liquid glue, stirring makes it completely dissolved, and obtains the liquid glue containing nitroguanidine；Under 35 DEG C of temperature conditions, TKX 50 is added in fluid bed granulation unit, after persistently mixing 40min, liquid glue containing nitroguanidine is sprayed into the fluosolids of fluid bed granulation unit, after carrying out mixing granulation, it is dry in fluid bed granulation unit under the conditions of 40 DEG C of temperature, the TKX 50 that nitroguanidine is granulated after cladding is obtained after sieving；Preparation process of the present invention is simple, and preparation process adds and subtracts pressure device without high temperature, and solvent for use is repeatable to be recycled.Product yield is higher, and the yield that fluidization spray obtained is granulated the TKX 50 after cladding is 99%~99.99%, and the grain graininess of gained is uniform, and mobility, press formability are good.
Description
Technical field
The present invention relates to a kind of methods that nitroguanidine fluidization spray is granulated cladding TKX-50, belong to energetic material field.
Background technology
It efficiently injures and explosive strength performance requirement is continuously improved, Modern weapon system requires energetic material that must have energy
The high and low vulnerability of metric density and it is safe the features such as.1,1'- dihydroxy -5,5'- bistetrazole dihydroxy amine salt (hereinafter referred to as TKX-
50) be a kind of novel high-energy single chmical compound explosive, be white crystals graininess high-energy, low sensitivity tetrazolium containing can ion salt, be close
The novel energetic material that year occurs, due to energy height, by application field extensive concern.Numerous composite explosives documents do not have substantially
It was found that document in terms of the composite explosives with TKX-50, the optimization of the synthetic technological condition in relation to TKX-50 and the theoretical calculation of formula
More typically.The insensitiveness covering material of TKX-50 not only influences the explosion property of composite explosives, while also influencing the compatibility of explosive,
Method now is used to coat TKX-50 after-explosions performance and mechanical property and requirement using department is not achieved.Explosive passivation packet
Coating technique mainly has high molecular polymer cladding, composite material cladding process, passivation nitro compounds to live as deterrent cladding process, surface
The methods of property agent.Wherein, other technologies are better than using composite material coated explosive effect, high-quality advanced composite explosives are to material
Compatibility and it is compound after the performance of explosive is influenced it is more demanding.
Nitroguanidine (NQ) is a kind of white needle-like crystals that extremely low mechanical sensitivity is 0%, be can be used as blunt in composite explosives
Agent, but have no document report in terms of insensitiveness TKX-50.The present invention is granulated cladding TKX-50 with nitroguanidine fluidization spray.Fluidisation
During mist projection granulating, material powders keep the fluidized state to suspend, liquid viscous under the airflow function in container from bottom to top
Mixture makes powder be agglomerated into particle to fluosolids penetrating, and mixing, granulation, dry 3 steps are once completed in closed container, and
The overall process of granulation is only influenced by bed interior air-flow not by outer force effect, therefore grain density obtained is small, and particle intensity is low, but institute
The grain graininess obtained is uniform, and mobility, compressibility are good.
Invention content
The object of the present invention is to provide a kind of method that nitroguanidine fluidization spray is granulated cladding TKX-50, this method can drop
The sensitivity of low TKX-50 improves powder charge performance, while improving powder charge safety and powder charge is molded, does not influence its energy water
It is flat.
The purpose of the present invention is what is be achieved through the following technical solutions.
A kind of method that nitroguanidine fluidization spray is granulated cladding TKX-50, is as follows：
Step 1: in 20~70 DEG C of temperature, under 150~300r/min mixing speeds, adhesive is added to anhydrous solvent
In, keep temperature-resistant, stirring obtains the liquid glue that mass fraction is 0.5%~0.8% up to being completely dissolved；
Step 2: nitroguanidine is added in liquid glue made from step 1, under the conditions of 40~50 DEG C, with 100~
The stirring of 200r/min mixing speeds makes it completely dissolved, and obtains the liquid glue containing nitroguanidine；
Step 3: under 15~35 DEG C of temperature conditions, TKX-50 is added in fluid bed granulation unit, persistently mixes 20
After~40min, the liquid glue containing nitroguanidine that step 2 obtains is sprayed into the fluosolids of fluid bed granulation unit, is mixed
It closes and is granulated 20~50min, the TKX-50 crude products after being coated；
Step 4: the TKX-50 crude products sieving after the cladding that step 3 obtains, dry under the conditions of 15~60 DEG C of temperature
Whole grain is carried out after 2h~8h, obtains the TKX-50 that nitroguanidine is granulated after cladding；
The addition mass ratio of the adhesive, nitroguanidine and TKX-50 is (0.5~1.5)：(1~10)：100；
Adhesive described in step 1 is polyvinyl butyral, polyacrylic acid, polymethyl acrylate and polymethyl
One kind in sour methyl esters；
Anhydrous solvent described in step 1 is any one in ethyl acetate, acetone and ethyl alcohol；
The grain size of TKX-50 described in step 3 is 100~300 mesh；
The grain size being sieved described in step 4 is 100~300 mesh.
Advantageous effect
1, the method that a kind of nitroguanidine fluidization spray of the invention is granulated cladding TKX-50, production preparation facilities is simple, system
Standby operation simple for process, preparation process add and subtract pressure device without high temperature, and solvent for use is repeatable to be recycled, and environmental requirement is met,
Safe operation is reliable simultaneously, and industrialized production may be implemented.
2, the method that a kind of nitroguanidine fluidization spray of the invention is granulated cladding TKX-50, product yield obtained is higher,
The yield that fluidization spray made from the product is granulated the TKX-50 after cladding is 99%~99.99%, and the grain graininess of gained is equal
Even, mobility, press formability are good.
3, the method that a kind of nitroguanidine fluidization spray of the invention is granulated cladding TKX-50, products obtained therefrom friction and shock sense
Spend energy level that is low, while not influencing product.
Specific implementation mode
Present disclosure is described further in conjunction with the embodiments.
Embodiment 1
Under 70 DEG C, 300r/min mixing speeds, 5g polyvinyl butyrals are added in 800g ethyl acetate, are kept
Temperature-resistant, stirring makes it completely dissolved, and obtains the liquid glue that mass fraction is 0.62%；At 50 DEG C, stirred with 200r/min
Under velocity conditions, 50g nitroguanidines are added in aforesaid liquid glue, stirring makes it completely dissolved, and obtains the liquid containing nitroguanidine
Body glue；Under 35 DEG C of temperature conditions, the 945gTKX-50 that grain size is 230 mesh is added in fluid bed granulation unit, is persistently mixed
After closing 40min, the liquid glue containing nitroguanidine is sprayed into the fluosolids of fluid bed granulation unit, carries out mixing granulation
After 50min, under the conditions of 40 DEG C of temperature, dry 4h, nitroguanidine is obtained after being sieved with 200 mesh sieve in fluid bed granulation unit
The TKX-50 being granulated after cladding；
The TKX-50 white particle product 991g that nitroguanidine is granulated after cladding are obtained, it is general to hit explosion for yield 99.1%
Rate is 10% (10kg drops hammer), and characteristic drop height is 22cm (25kg drops hammer), and friction explosion probability is 9% (3.92M Pa, 90 °),
Explosion velocity 9045m/s (ρ=1.811g/cm3)。
Embodiment 2
At 55 DEG C of temperature, 200r/min mixing speeds, 0.6g polymethyl acrylate is added in 80g ethyl alcohol, is kept
Temperature-resistant, stirring makes it completely dissolved, and obtains the liquid glue that mass fraction is 0.74%；At 45 DEG C, 180r/min stirrings are fast
Under the conditions of degree, 5g nitroguanidines are added in 80g liquid glues, stirring makes it completely dissolved, and obtains the liquid glue containing nitroguanidine；
Under 30 DEG C of temperature conditions, the 94.4gTKX-50 that grain size is 200 mesh is added in fluid bed granulation unit, it is lasting to mix
After 35min, the liquid glue containing nitroguanidine is sprayed into the fluosolids of fluid bed granulation unit, carries out mixing granulation 40min
Afterwards, under the conditions of temperature 50 C, the dry 2h in fluid bed granulation unit obtains nitroguanidine and is granulated after being sieved with 230 mesh sieve
TKX-50 after cladding；
The TKX-50 white particle product 99.4g that nitroguanidine is granulated after cladding are obtained, it is general to hit explosion for yield 99.4%
Rate is 10% (10kg drops hammer), and characteristic drop height is 23cm (25kg drops hammer), and friction explosion probability is 7% (3.92M Pa, 90 °),
Explosion velocity 9021m/s (ρ=1.806g/cm3)。
Embodiment 3
Under temperature 60 C, 190r/min mixing speeds, 0.5g polyacrylic acid is added in 75g ethyl alcohol, keeps temperature not
Become, stirring makes it completely dissolved, and obtains the liquid glue that mass fraction is 0.66%；At 40 DEG C, 180r/min mixing speed conditions
Under, 5.5g nitroguanidines are added in 75g liquid glues, stirring makes it completely dissolved, and obtains the liquid glue containing nitroguanidine；35
Under DEG C temperature condition, by 94 grams of TKX-50 that grain size is 260 mesh and it is added in fluid bed granulation unit, persistently mixes 35min
Afterwards, the liquid glue containing nitroguanidine is sprayed into the fluosolids of fluid bed granulation unit, after carrying out mixing granulation 40min,
Under the conditions of 15 DEG C of temperature, the dry 8h in fluid bed granulation unit, after nitroguanidine granulation cladding is obtained after being sieved with 200 mesh sieve
TKX-50；
The TKX-50 white particle product 99.3g that nitroguanidine is granulated after cladding are obtained, it is general to hit explosion for yield 99.3%
Rate is 9% (10kg drops hammer), and characteristic drop height is 21cm (25kg drops hammer), and friction explosion probability is 8% (3.92M Pa, 90 °), quick-fried
Fast 9048m/s (ρ=1.812g/cm3)。
Embodiment 4
At 65 DEG C of temperature, 180r/min mixing speeds, 0.7g polymethyl methacrylates are added to 90g acetone, are protected
Hold temperature-resistant, stirring makes it completely dissolved, and obtains the liquid glue that mass fraction is 0.77%；At 48 DEG C, 175r/min is stirred
Under velocity conditions, 7g nitroguanidines are added in 75g liquid glues, stirring makes it completely dissolved, and obtains the liquid containing nitroguanidine
Glue；Under 25 DEG C of temperature conditions, grain size for 92.3 grams of TKX-50 of 260 mesh and is added in fluid bed granulation unit, is continued
After mixing 30min, the liquid glue containing nitroguanidine is sprayed into the fluosolids of fluid bed granulation unit, carries out mixing granulation
After 45min, under the conditions of temperature 50 C, dry 3h, nitroguanidine is obtained after being sieved with 200 mesh sieve in fluid bed granulation unit
The TKX-50 being granulated after cladding；
The TKX-50 white particle product 99.4g that nitroguanidine is granulated after cladding are obtained, it is general to hit explosion for yield 99.4%
Rate is 12% (10kg drops hammer), and characteristic drop height is 24cm (25kg drops hammer), and friction explosion probability is 6% (3.92M Pa, 90 °),
Explosion velocity 9037m/s (ρ=1.809g/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 above is only a specific embodiment of the present invention, for explaining the present invention, being not used to limit this
The protection domain of invention, all within the spirits and principles of the present invention, any modification, equivalent substitution, improvement and etc. done should all
It is included within protection scope of the present invention.
Claims (6)
1. a kind of method that nitroguanidine fluidization spray is granulated cladding TKX-50, it is characterised in that：It is as follows：
Step 1: in 20~70 DEG C of temperature, under 150~300r/min mixing speeds, adhesive is added in anhydrous solvent, is protected
Hold temperature-resistant, stirring obtains the liquid glue that mass fraction is 0.5%~0.8%, liquid glue is positioned over until be completely dissolved
It is spare under the conditions of 20~50 DEG C；
Step 2: nitroguanidine is added in liquid glue made from step 1, under the conditions of 40~50 DEG C, with 100~200r/
The stirring of min mixing speeds makes it completely dissolved, and obtains the liquid glue containing nitroguanidine；
Step 3: under 15~35 DEG C of temperature conditions, TKX-50 is added in fluid bed granulation unit, persistently mix 20~
After 40min, the liquid glue containing nitroguanidine that step 2 obtains is sprayed into the fluosolids of fluid bed granulation unit, is mixed
It is granulated 20~50min, the TKX-50 crude products after being coated；
Step 4: the TKX-50 crude products sieving after the cladding that step 3 obtains, under the conditions of 15~60 DEG C of temperature dry 2h~
Whole grain is carried out after 8h, obtains the TKX-50 that nitroguanidine is granulated after cladding.
2. the method that a kind of nitroguanidine fluidization spray as described in claim 1 is granulated cladding TKX-50, it is characterised in that：It is described
The addition mass ratio of adhesive, nitroguanidine and TKX-50 is (0.5~1.5)：(1~10)：100.
3. the method that a kind of nitroguanidine fluidization spray as described in claim 1 is granulated cladding TKX-50, it is characterised in that：Step
Adhesive described in one is one in polyvinyl butyral, polyacrylic acid, polymethyl acrylate and polymethyl methacrylate
Kind.
4. the method that a kind of nitroguanidine fluidization spray as described in claim 1 is granulated cladding TKX-50, it is characterised in that：Step
Anhydrous solvent described in one is any one in ethyl acetate, acetone and ethyl alcohol.
5. the method that a kind of nitroguanidine fluidization spray as described in claim 1 is granulated cladding TKX-50, it is characterised in that：Step
The grain size of TKX-50 described in three is 100~300 mesh.
6. the method that a kind of nitroguanidine fluidization spray as described in claim 1 is granulated cladding TKX-50, it is characterised in that：Step
The grain size being sieved described in four is 100~300 mesh.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| 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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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| 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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| Publication Number | Publication Date |
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| CN108558587A true CN108558587A (en) | 2018-09-21 |
| CN108558587B CN108558587B (en) | 2020-09-18 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116924862A (en) * | 2022-03-29 | 2023-10-24 | 南京理工大学 | Application of KH550 coated TKX-50 in improving nitrocotton compatibility |
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 |
-
2018
- 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 |
Non-Patent Citations (1)
| Title |
|---|
| 欧育湘: "《炸药学》", 28 February 2014, 北京理工大学出版社 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116924862A (en) * | 2022-03-29 | 2023-10-24 | 南京理工大学 | Application of KH550 coated TKX-50 in improving nitrocotton compatibility |
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